CN105548043A - Method for rapid determination of polymerization rate of ammonium polyphosphate-containing fertilizer sample - Google Patents

Method for rapid determination of polymerization rate of ammonium polyphosphate-containing fertilizer sample Download PDF

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Publication number
CN105548043A
CN105548043A CN201510919589.XA CN201510919589A CN105548043A CN 105548043 A CN105548043 A CN 105548043A CN 201510919589 A CN201510919589 A CN 201510919589A CN 105548043 A CN105548043 A CN 105548043A
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sample
orthophosphate
phosphorus
content
tested
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CN105548043B (en
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谷焕芝
褚红艳
刘腾
戴毅平
张建军
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Shenzhen Batian Ecotypic Engineering Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry

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  • Health & Medical Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
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Abstract

The invention provides a method for rapid determination of the polymerization rate of an ammonium polyphosphate-containing fertilizer sample, wherein the method comprises the steps: drawing a standard curve according to the relationship between the content and the absorbance of a standard material; adjusting the acid-base value of a to-be-tested sample; adding acetone to the to-be-tested sample, freezing, then adding ammonium molybdate, carrying out a reaction with orthophosphate to generate a complex, making the volume constant, then controlling the indoor temperature and humidity, and determining the content of phosphorus in orthophosphate; then taking the to-be-tested sample, making the volume constant, then filtering, adding a nitric acid solution, heating to boil, cooling, then adding acetone, freezing, adding ammonium molybdate, making the volume constant, controlling the indoor temperature and humidity, and determining the content of water soluble phosphorus; and finally, calculating the polymerization rate y according to the data comprising the phosphorus content of orthophosphate and the content of the water soluble phosphorus. Through control of the acid-base value of the sample and determination of the temperature and humidity of the environment, the hydrolysis velocity of the sample solution is alleviated, the problems of cuvette fogging and acetone volatilization in the determination process are solved, the accuracy of the testing is effectively improved, and the deviation of the final determination result is less than 5%.

Description

Fast Measurement is containing the method for APP fertilizer sample aggregate rate
Technical field
The invention belongs to fertilizer technical field of measurement and test, particularly relate to a kind of can Fast Measurement containing the method for APP fertilizer sample aggregate rate.
Background technology
The domestic assay method for containing APP fertilizer is not sought unity of standard at present, and is an important indicator to the detection containing polyphosphoric acid ammonia fertilizer material aggregate rate, so it is very important to seek the method that accurately can detect aggregate rate.In prior art, the method detected for APP aggregate rate has paper chromatography, ion exchange process, colourimetry, high performance liquid chromatography.
The ultimate principle mentioning ion exchange process in the ion chromatography analysis research of the polyphosphate that the people such as Song Xiuxian deliver is: sample makes the APP of different polymerization degree separate by ion exchange column, orthophosphate is first eluted, large rear of the degree of polymerization is eluted, according to eluting the amount of orthophosphate and calculating aggregate rate with the gauge of the water-soluble phosphorus of gravimetric determination.But this method due to the composition contained in fertilizer more, ion composition more complicated, when carrying out wash-out with strong anion exchange resin, the existence of other ion can be disturbed and align phosphatic wash-out, causes experimental result inaccurate.This is because except containing phosphate anion in fertilizer, also containing other ion, composition relative complex, the existence of some ion can affect eluant, eluent and align phosphatic wash-out, finally causes measurement result inaccurate.
High performance liquid chromatography: the high performance liquid chromatography measuring high performance liquid chromatography molecular chain conformation is a kind of means measuring the molecular chain conformation of polymer substance fast and automatically.The propositions such as ChikashiFukumura, with the high performance liquid chromatograph that waters company limited makes, and make with the polyglycol of different molecular weight and polyoxyethylene the typical curve drenching volume-molecular weight, record the molecular chain conformation of APP, and then calculate the aggregate rate of APP.But this method lacks the polyglycol of various fraction molecular weight and the sample of polyoxyethylene when doing typical curve, and chromatographic column fixed phase is not easily selected, add high performance liquid chromatograph price costly, cost is higher, when doing typical curve, sample not easily obtains, and also there is larger difficulty when selecting Stationary liquid, so be not suitable as the common method that aggregate rate detects in enterprise.
Paper chromatography: adopt paper chromatography method to carry out the separation of each component in APP, wash-out is also hydrolyzed rear and ammonium molybdate reaction, then with reductive agent reduction, surveys absorbance, calculate the aggregate rate of APP according to the absorbance of each component at 650nm place.Easily there is conditions of streaking in this method, cause each Component seperation poor effect, affect final measurement result, and test period is longer in expansion process.The organic reagent that paper chromatography is used is toxic, and Long Term Contact is harmful to health.
Colourimetry: colourimetry is also called express method, principle gets orthophosphate in fertilizer and Quadrafos by water extraction, orthophosphate and ammonium molybdate effect generate yellow complex, its absorbance is measured at wavelength 430nm place, the content of phosphorus pentoxide in water-soluble orthophosphate is calculated according to absorbance, and then calculate the aggregate rate of sample, but still there is the inaccurate problem of final measurement result in this method in practical operation.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art, provide the method for a kind of Fast Measurement containing APP fertilizer sample aggregate rate, in order to solve the inaccurate problem of measurement result in colorimetric method for determining.
A kind of Fast Measurement provided by the invention, containing the method for APP fertilizer sample aggregate rate, comprises the steps:
According to the relation drawing standard curve between the content of standard substance and absorbance;
Regulate sample to be tested potential of hydrogen;
Measure phosphorus content in the orthophosphate in sample to be tested: in sample to be tested, add a certain amount of acetone, after freezing, add ammonium molybdate, with constant volume after orthophosphate reacting generating complex, control indoor temperature and relative humidity, then measure;
Measure the content of water-soluble phosphorus in sample to be tested: filter after getting a certain amount of sample to be tested constant volume, get appropriate filtrate in beaker, add salpeter solution heating to boil, get appropriate in volumetric flask after cooling, add acetone freezing, add ammonium molybdate constant volume, control indoor temperature and relative humidity, then measure;
According to the orthophosphate phosphorus content of above-mentioned acquisition, the data of water-soluble phosphorus content, according to following formulae discovery aggregate rate y:
y = x 1 - x 2 x 1 × 100
In formula: water-soluble phosphorus content in X1----sample
Phosphorus content in orthophosphate in X2-----sample.
The present invention is by controlling the potential of hydrogen of sample to be tested, alleviate the hydrolysis rate of sample solution, simultaneously by controlling the temperature and humidity measuring environment, solve the problem that cuvette in mensuration process hazes and acetone volatilizees, the accuracy of testing effectively is improved, its final measurement result deviation is within 5%, and the test duration is short, and the reappearance of experiment is better.
Accompanying drawing explanation
Fig. 1 is method of testing FB(flow block) of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
See Fig. 1, the invention provides the method for a kind of Fast Measurement containing APP fertilizer sample aggregate rate, comprise the steps:
S1: according to the relation drawing standard curve between the content of standard substance and absorbance.Specifically standard solution can be drawn in 50ml volumetric flask, add acetone and carry out freezing 20 minutes, then add constant volume after 4ml-5ml ammonium molybdate solution, control indoor temperature less than 20 DEG C, indoor relative humidity below 55, in 430nm place mensuration absorbance.
In Experiment of Analytical Chemistry, calibration curve method usually often can be used to carry out quantitative test, this is a kind of easy, quantivative approach fast, can according to the relation drawing standard curve between the content of standard substance and absorbance.After the present invention adopts standard substance drawing standard curve, the orthophosphate after can measuring and water-soluble phosphorus content, finally just can calculate aggregate rate according to the content meter measured.
S2: regulate sample to be tested potential of hydrogen.A certain amount of sample can be taken, add alkali compounds in advance, make its pH value between 7.5-8.5, the hydrolysis rate of sample to be tested can be alleviated, ensure the accuracy of test.In this step, the alkali added should ensure not react with the material in system, can not be mixed with composition to be measured, preferred inorganic base, because inorganic base composition is relatively simple, not easily brings other impurity component into, can select NaOH, potassium hydroxide etc.
S3: measure phosphorus content in the orthophosphate in sample to be tested.Above-mentioned steps potpourri is filtered, then get a certain amount of in 50ml volumetric flask, add a certain amount of acetone, after the time of freezing one, add ammonium molybdate constant volume, with constant volume after orthophosphate reacting generating complex, control indoor temperature 10-20 DEG C, indoor relative humidity at 45-55, then measure.
In described S3 step, acetone can play the effect suppressing APP hydrolysis in sample to be tested, the general acetone adding 25ml in 50ml volumetric flask, add acetone and too much affect accuracy of measurement, the very few effect not having suppression hydrolysis, the acetone weight generally added accounts for about the 40%-60% of sample to be tested weight.After freezing 20-30min, add ammonium molybdate, with orthophosphate reacting generating complex, such complex compound can record its absorbance and concentration on ultraviolet spectrophotometer.Generally in 50ml volumetric flask, add 4-6ml ammonium molybdate solution, addition is the 5%-10% of sample to be tested weight, and it is incomplete to add very few orthophosphate and its reaction, adds and too much can affect accuracy of measurement.
In this step, add a certain amount of acetone in the sample, solve the problem of the measurement result error that sample causes because of hydrolysis, control temperature and humidity during reaction simultaneously, solve acetone volatilization and affect measurement result and the surperficial problem making measurement result higher that hazes of cuvette soon, thus improve the accuracy of test.
S4: the content measuring water-soluble phosphorus in sample to be tested: water-soluble phosphorus comprises the mensuration of orthophosphate, metaphosphate, pyrophosphate, polyphosphate, filter after desirable a certain amount of sample to be tested constant volume, then appropriate filtrate is got in 500ml beaker, add salpeter solution heating to boil, get appropriate in 50ml volumetric flask after cooling, it is freezing to add acetone, adds ammonium molybdate constant volume, control indoor temperature 10-20 DEG C, indoor relative humidity at 45-55 degree, then measure;
In described S4 step, measure the content of water-soluble phosphorus, essence is the content of phosphorus pentoxide in solution, i.e. the quality of phosphorus pentoxide in every ml soln, and unit is ug/ml.Nitric acid in this step and water volume ratio are 0.4-0.6:1, are mixed to get described salpeter solution.The addition of described acetone is the 40%-60% of sample to be tested weight, can add the acetone of 25ml in 50ml volumetric flask.
Similarly, this step adds acetone, is also to play the effect suppressing APP hydrolysis, and adding acetone too much affects accuracy of measurement, the very few effect not having suppression hydrolysis.Meanwhile, control temperature and humidity during reaction, solving acetone volatilization affects measurement result and the surperficial problem making measurement result higher that hazes of cuvette soon, improves the accuracy of test equally.
S5: according to the data of phosphorus pentoxide content in phosphorus content, water-soluble phosphorus in the orthophosphate of above-mentioned acquisition, according to following formulae discovery aggregate rate y:
y = x 1 - x 2 x 1 × 100
Phosphorus pentoxide content in water-soluble phosphorus in X1----sample
Phosphorus content in orthophosphate in X2-----sample.
Phosphorus content X2 in phosphorus pentoxide content X1, orthophosphate in water-soluble phosphorus in the sample of said determination is substituted into above-mentioned formula, just can obtain the aggregate rate percent value containing APP fertilizer sample.
The invention described above measures the method containing APP fertilizer sample aggregate rate, by regulating the potential of hydrogen of sample to be tested before the assay, alleviate the hydrolysis rate in sample solution test process, add the effect that acetone suppresses APP hydrolysis simultaneously, and by limiting the temperature and humidity measuring environment, both the environmental requirement of mensuration had been met, it also avoid acetone to volatilize soon and the surperficial phenomenon that hazes of cuvette simultaneously, make measurement result deviation within 5%, improve the accuracy adopting colorimetric method for determining aggregate rate, and it is better to test reappearance.
Embodiment:
S1: the preparation of standard solution and Specification Curve of Increasing:
(1). first prepare phosphorus standard reserving solution:
Dissolve 1.9157g and dry the potassium dihydrogen phosphates of two hours in water at 105 DEG C in advance, be settled to 1L, this solution phosphorus pentoxide concentration is 1mg/ml;
(2). prepare phosphorus standard solution with phosphorus standard reserving solution: accurately pipette phosphorus standard reserving solution in 10ml step (1) in 100ml volumetric flask, be settled to 100ml, this solution is standard solution, and the concentration of this solution is 0.1mg/ml.
(3) get in standard solution 0ml, the 5ml of known phosphorus content, 10ml, 15ml, 20ml to 50ml volumetric flask respectively, then add 25ml, concentration 99.5% analyzes pure acetone and carry out freezing 20 minutes, and then in each volumetric flask, add the ammonium molybdate solution 4ml constant volume that concentration is 37.6mg/ml, control indoor temperature about 20 DEG C, indoor relative humidity at about 55 degree, 430nm place mensuration absorbance.Ultraviolet-visible pectrophotometer is adopted to determine the absorbance of surveyed solution, then according to the relation automatic Fitting curve between the phosphorus content of known standard solution and the absorbance determining solution and fitting equation.
S2: the sample taking 2ml, then adds 1ml, concentration is 1mg/ml NaOH, stirs, makes its pH value about 8.
S3: the potpourri of above-mentioned steps is filtered, then the acetone of 25ml is got in 50ml volumetric flask, after freezing 20min, adding concentration is 37.6mg/ml ammonium molybdate 4ml constant volume, with constant volume after orthophosphate reacting generating complex, control indoor temperature 20 DEG C, indoor relative humidity at 55 degree, then in mensuration sample, phosphorus content X2 is 14.2867% in orthophosphate.
S4: get 100mg-200mg to filter after the sample constant volume of phosphorus pentoxide, then 25ml filtrate is got in 500ml beaker, add the heating of 10ml salpeter solution to boil, be cooled to room temperature, get 2ml in 50ml volumetric flask, after adding the freezing 20min of acetone 25ml, adding concentration is 37.6mg/ml ammonium molybdate 4ml constant volume, control indoor temperature 20 DEG C, indoor relative humidity at 55 degree, then carrying out the content X1 of phosphorus pentoxide in mensuration sample is 28.5946%;
S5: according to the data of phosphorus pentoxide content X1 in phosphorus content X2, water-soluble phosphorus in the orthophosphate of above-mentioned acquisition, according to following formulae discovery aggregate rate y:
y = x 1 - x 2 x 1 × 100
X1＝28.5946％，X2＝14.2867％
y = x 1 - x 2 x 1 × 100 = 28.5946 - 14.2867 28.5946 × 100 = 50.04 %
From above-mentioned result of calculation, the aggregate rate adopting method of testing of the present invention to obtain is 50.04%, and its aggregate rate known is 50%, and its deviation is within 5%.
Following list is 4 samples of known aggregate rate, adopts the colorimetric method for determining aggregate rate of prior art and adopts the correlation data of colorimetric method for determining aggregate rate of the present invention.
From above-mentioned correlation data, the aggregate rate result adopting the present invention to measure is more accurate, and deviation is within 5%.
In sum; be only the part of present pre-ferred embodiments shown in the above embodiment of the present invention, the present invention can not be limited to this, under the condition not departing from marrow of the present invention; any amendment that those skilled in the art do, equivalent replacement and improvement etc., all belong to protection scope of the present invention.

Claims (9)

1. Fast Measurement is containing a method for APP fertilizer sample aggregate rate, it is characterized in that, comprises the steps:
According to the relation drawing standard curve between the content of standard substance and absorbance;
Regulate sample to be tested potential of hydrogen;
Measure phosphorus content in the orthophosphate in sample to be tested: in sample to be tested, add a certain amount of acetone, after freezing, add ammonium molybdate, with constant volume after orthophosphate reacting generating complex, control indoor temperature and relative humidity, then measure;
Measure the content of water-soluble phosphorus in sample to be tested: filter after getting a certain amount of sample to be tested constant volume, get appropriate filtrate in beaker, add salpeter solution heating to boil, get appropriate in volumetric flask after cooling, add acetone freezing, add ammonium molybdate constant volume, control indoor temperature and relative humidity, then measure;
According to the orthophosphate phosphorus content of above-mentioned acquisition, the data of water-soluble phosphorus content, according to following formulae discovery aggregate rate y:
y = x 1 - x 2 x 1 × 100
In formula: water-soluble phosphorus content in X1----sample
Phosphorus content in orthophosphate in X2-----sample.
2. Fast Measurement as claimed in claim 1 is containing the method for APP fertilizer sample aggregate rate, it is characterized in that, the step of described drawing standard curve draws standard solution in 50ml volumetric flask, add acetone freezing 20 minutes, add constant volume after 4ml ammonium molybdate solution, control indoor temperature less than 20 DEG C, indoor relative humidity below 55 degree, 430nm place mensuration absorbance.
3. Fast Measurement as claimed in claim 1 is containing the method for APP fertilizer sample aggregate rate, it is characterized in that, selects inorganic base to regulate described sample to be tested potential of hydrogen, regulates ph between 7.5-8.5.
4. Fast Measurement as claimed in claim 1 is containing the method for APP fertilizer sample aggregate rate, and it is characterized in that, in described orthophosphate in phosphorus detection step, indoor temperature controls at 10-20 DEG C, and indoor relative humidity controls at 45-55 degree.
5. Fast Measurement as claimed in claim 1 is containing the method for APP fertilizer sample aggregate rate, and it is characterized in that, in the assay step of described water-soluble phosphorus, indoor temperature controls at 10-20 DEG C, and indoor relative humidity controls at 45-55 degree.
6. the Fast Measurement as described in any one of claim 1-5 is containing the method for APP fertilizer sample aggregate rate, and it is characterized in that, in described orthophosphate in phosphorus detection step, the addition of described acetone is the 40%-60% of sample to be tested weight.
7. the Fast Measurement as described in any one of claim 1-5 is containing the method for APP fertilizer sample aggregate rate, and it is characterized in that, in described orthophosphate in phosphorus detection step, the addition of described ammonium molybdate is the 5%-10% of sample to be tested weight.
8. the Fast Measurement as described in any one of claim 1-5 is containing the method for APP fertilizer sample aggregate rate, and it is characterized in that, in the assay step of described water-soluble phosphorus, described salpeter solution concentration is 40%-60%.
9. the Fast Measurement as described in any one of claim 1-5 is containing the method for APP fertilizer sample aggregate rate, and it is characterized in that, in the assay step of described water-soluble phosphorus, the addition of described acetone is the 40%-60% of sample to be tested weight.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106442473A (en) * 2016-08-31 2017-02-22 瓮福达州化工有限责任公司 Detection method of element content in compound fertilizer
CN108254369A (en) * 2018-02-08 2018-07-06 什邡市长丰化工有限公司 A kind of detection method of water-soluble poly ammonium phosphate aggregate rate
CN111337444A (en) * 2020-04-17 2020-06-26 大连理工大学 Method for detecting whether vaccine is frozen or not by using ultraviolet spectrophotometer

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106442473A (en) * 2016-08-31 2017-02-22 瓮福达州化工有限责任公司 Detection method of element content in compound fertilizer
CN108254369A (en) * 2018-02-08 2018-07-06 什邡市长丰化工有限公司 A kind of detection method of water-soluble poly ammonium phosphate aggregate rate
CN111337444A (en) * 2020-04-17 2020-06-26 大连理工大学 Method for detecting whether vaccine is frozen or not by using ultraviolet spectrophotometer

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