CN105548043B - The method of the quick measure aggregate rate of fertilizer sample containing APP - Google Patents
The method of the quick measure aggregate rate of fertilizer sample containing APP Download PDFInfo
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- CN105548043B CN105548043B CN201510919589.XA CN201510919589A CN105548043B CN 105548043 B CN105548043 B CN 105548043B CN 201510919589 A CN201510919589 A CN 201510919589A CN 105548043 B CN105548043 B CN 105548043B
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- 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
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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Abstract
The invention provides a kind of method of the quick measure aggregate rate of fertilizer sample containing APP, it is：Standard curve is drawn according to the relation between the content and absorbance of standard substance；Adjust sample to be tested acid-base value；Ammonium molybdate is added after acetone freezing is added in sample to be tested, with temperature and humidity in constant volume, then control room after orthophosphates reaction generation complex compound, determines phosphorus content in orthophosphates；Then filtered after taking sample to be tested constant volume, add salpeter solution heating and boil, addition acetone freezes after cooling, ammonium molybdate constant volume, temperature and humidity in control room, determines the content of water-soluble phosphorus；Finally aggregate rate y is calculated according to the data of orthophosphates phosphorus content, water-soluble phosphorus content.The present invention passes through the acid-base value of Control Assay and the temperature and humidity of determination of the environment, alleviate the hydrolysis rate of sample solution, solve the problems, such as that cuvette hazes and acetone volatilization in continuous mode so that the accuracy of test effectively improves, and final measurement result deviation is within 5%.
Description
Technical field
The invention belongs to fertilizer technical field of measurement and test, more particularly to one kind can quickly determine fertilizer sample containing APP and gather
The method of conjunction rate.
Background technology
The domestic assay method for the fertilizer containing APP is not sought unity of standard at present, and the material of ammonia fertilizer containing polyphosphoric acid is gathered
The detection of conjunction rate is an important indicator, thus seek can accurately detect aggregate rate method it is particularly significant.In the prior art,
There are paper chromatography, ion-exchange, colorimetric method, high performance liquid chromatography for the method for APP aggregate rate detection.
The basic of ion-exchange is mentioned in the ion chromatography analysis research of virtuous et al. the polyphosphates delivered of Song Xiu
Principle is：Sample separates the APP of different polymerization degree by ion exchange column, and orthophosphates is first eluted out, polymerization
It is eluted out after degree is big, polymerization is calculated according to the amount for eluting orthophosphates and with the gauge of the water-soluble phosphorus of gravimetric detemination
Rate.But this method, because the composition contained in fertilizer is more, ion composition is more complicated, is carried out with strong anion exchange resin
During elution, the presence of other ions, which can be disturbed, aligns phosphatic elution, causes experimental result inaccurate.Because in fertilizer
Except containing phosphate anion, also containing other ions, composition is relative complex, and the presence of some ions can influence eluant, eluent and align
Phosphatic elution, ultimately cause measurement result inaccuracy.
High performance liquid chromatography：The high performance liquid chromatography of measure high performance liquid chromatography molecular chain conformation is a kind of fast
The means of molecular chain conformation that is fast, automatically determining polymer substance.Chikashi Fukumura etc. are proposed, are had with waters
The high performance liquid chromatograph that limit company makes, and make of the polyethylene glycol and polyethylene glycol oxide of different molecular weight drench volume-
The standard curve of molecular weight, has measured the molecular chain conformation of APP, and then calculates the aggregate rate of APP.But this
Kind method lacks the polyethylene glycol of various fraction molecular weights and the sample of polyethylene glycol oxide, and chromatographic column when doing standard curve
Stationary phase is not easy to select, and plus high performance liquid chromatograph price costly, cost is higher, and when doing standard curve, sample is not easy to obtain
Take, and when selecting stationary phase there is also larger difficulty, so it is not suitable as the common method of enterprise's detection aggregate rate.
Paper chromatography：Using paper chromatography method carry out APP in each component separation, after eluting and hydrolyzing with molybdic acid
Ammonium is reacted, then is reduced with reducing agent, and absorbance is surveyed at 650nm, and the poly- of APP is calculated according to the absorbance of each component
Conjunction rate.Easily there is conditions of streaking during expansion in this method, causes each component separating effect bad, influences final measure knot
Fruit, and test period is longer.The organic reagent that paper chromatography is used is toxic, and Long Term Contact is harmful to body.
Colorimetric method：Colorimetric method is also known as express method, and principle is that the orthophosphates and Quadrafos in fertilizer are extracted with water, just
Phosphate and ammonium molybdate effect generation yellow complex, its absorbance is determined at wavelength 430nm, water outlet is calculated according to absorbance
The content of phosphorus pentoxide in dissolubility orthophosphates, and then the aggregate rate of sample is calculated, but this method is in practical operation
There are still the problem of final measurement result inaccuracy.
The content of the invention
It is an object of the invention to overcome deficiency of the prior art, there is provided a kind of quick measure fertilizer containing APP
The method of sample aggregate rate, to solve the problems, such as measurement result inaccuracy in colorimetric method for determining.
A kind of method of quick measure aggregate rate of fertilizer sample containing APP provided by the invention, comprises the steps：
Standard curve is drawn according to the relation between the content and absorbance of standard substance；
Adjust sample to be tested acid-base value；
Determine phosphorus content in the orthophosphates in sample to be tested：A certain amount of acetone is added in sample to be tested, after freezing
Ammonium molybdate is added, with constant volume, 10-20 DEG C of control indoor temperature and relative humidity 45-55 after orthophosphates reaction generation complex compound
Degree, is then measured；
Determine the content of water-soluble phosphorus in sample to be tested：Filtered after taking a certain amount of sample to be tested constant volume, take appropriate filtrate
In beaker, add salpeter solution heating and boil, taken after cooling in right amount in volumetric flask, add acetone freezing, add ammonium molybdate
Constant volume, 10-20 DEG C of control indoor temperature and relative humidity 45-55 degree, are then measured；
According to the orthophosphates phosphorus content of above-mentioned acquisition, the data of water-soluble phosphorus content, calculate and polymerize according to equation below
Rate y：
In formula：X1---- sample reclaimed water soluble phosphorus contents
Phosphorus content in orthophosphates in X2----- samples.
Acid-base value of the invention by controlling sample to be tested, the hydrolysis rate of sample solution is alleviated, while pass through control
The temperature and humidity of determination of the environment, solve the problems, such as that cuvette hazes in continuous mode and volatilized with acetone so that test
Accuracy effectively improves, and its final measurement result deviation is within 5%, and the testing time is short, and the reappearance of experiment is preferable.
Brief description of the drawings
Fig. 1 is method of testing FB(flow block) of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Referring to Fig. 1, the invention provides a kind of method of the quick measure aggregate rate of fertilizer sample containing APP, including under
State step：
S1：Standard curve is drawn according to the relation between the content and absorbance of standard substance.Specifically can be by standard liquid
Draw into 50ml volumetric flasks, add acetone and carry out freezing 20 minutes, then add constant volume after 4ml-5ml ammonium molybdate solutions, control
Indoor temperature processed is below 20 DEG C, indoor relative humidity below 55, at 430nm determine absorbance.
In Experiment of Analytical Chemistry, usually can often calibration curve method be used to carry out quantitative analysis, this is a kind of easy, quick
Quantitative approach, standard curve can be drawn according to the relation between the content and absorbance of standard substance.The present invention uses standard
After material draws standard curve, orthophosphates and water-soluble phosphorus content after can determining finally can be with containing according to measure
Gauge calculates aggregate rate.
S2：Adjust sample to be tested acid-base value.A certain amount of sample can be weighed, is previously added alkali compounds, makes 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 the step, the alkali of addition should be protected
Card does not react with the material in system, composition to be measured, preferably inorganic base can not be mixed with, because inorganic alkali composition is relatively simple
It is single, it is not easy to bring other impurity components into, sodium hydroxide, potassium hydroxide etc. may be selected.
S3：Determine phosphorus content in the orthophosphates in sample to be tested.Above-mentioned steps mixture is filtered, then taken a certain amount of
In 50ml volumetric flasks, a certain amount of acetone is added, after the time of one section of freezing, adds ammonium molybdate constant volume, it is anti-with orthophosphates
Constant volume after complex compound should be generated, control indoor temperature in 45-55, then determines in 10-20 DEG C, indoor relative humidity.
In the S3 steps, acetone can play a part of suppressing APP in sample to be tested and hydrolyze, and typically hold in 50ml
25ml acetone is added in measuring bottle, adding acetone excessively influences accuracy of measurement, very few not have the effect for suppressing hydrolysis, typically
The acetone weight of addition accounts for 40%-60% of sample to be tested weight or so.After freezing 20-30min, ammonium molybdate is added, with positive phosphorus
Hydrochlorate reaction generation complex compound, such complex compound can measure its absorbance and concentration on ultraviolet specrophotometer.Typically exist
4-6ml ammonium molybdate solutions are added in 50ml volumetric flasks, addition is the 5%-10% of sample to be tested weight, adds very few orthophosphoric acid
Salt reacts not exclusively, and addition can excessively influence accuracy of measurement.
In this step, a certain amount of acetone is added in the sample, solves sample because of measurement result caused by hydrolysis
The problem of error, while temperature and humidity when controlling reaction, it is fast and influence measurement result and colorimetric to solve acetone volatilization
Ware surface hazes so that the problem of measurement result is higher, so as to improve the accuracy of test.
S4：Determine the content of water-soluble phosphorus in sample to be tested：Water-soluble phosphorus includes orthophosphates, metaphosphate, pyrophosphoric acid
The measure of salt, polyphosphate, filtered after can use a certain amount of sample to be tested constant volume, then take appropriate filtrate in 500ml beakers
In, add salpeter solution heating and boil, taken after cooling in right amount in 50ml volumetric flasks, add acetone freezing, add ammonium molybdate and determine
Hold, control indoor temperature in 45-55 degree, is then measured in 10-20 DEG C, indoor relative humidity；
In the S4 steps, determine the content of water-soluble phosphorus, be substantially the content of phosphorus pentoxide in solution, i.e., every milliliter
The quality of phosphorus pentoxide in solution, unit ug/ml.Nitric acid and water volume ratio in the step are 0.4-0.6:1, mix
To described salpeter solution.The addition of the acetone is the 40%-60% of sample to be tested weight, can be added in 50ml volumetric flasks
Enter 25ml acetone.
Similarly, this step adds acetone, and plays a part of suppressing APP hydrolysis, and adding acetone excessively influences
Accuracy of measurement, it is very few not have the effect for suppressing hydrolysis.Meanwhile temperature and humidity when reacting is controlled, solve acetone and wave
Hair is fast and influences measurement result and cuvette surface hazes so that the problem of measurement result is higher, equally improves the standard of test
True property.
S5：According to the data of phosphorus pentoxide content in phosphorus content, water-soluble phosphorus in the orthophosphates of above-mentioned acquisition, according to such as
Lower formula calculates aggregate rate y：
Phosphorus pentoxide content in water-soluble phosphorus in X1---- samples
Phosphorus content in orthophosphates in X2----- samples.
By in phosphorus pentoxide content X1, orthophosphates in water-soluble phosphorus in the sample of said determination in phosphorus content X2 substitutions
Formula is stated, the aggregate rate percent value of the fertilizer sample containing APP can be obtained.
The method that the invention described above determines the aggregate rate of fertilizer sample containing APP, by adjusting sample to be tested before the assay
Acid-base value, alleviate the hydrolysis rate in sample solution test process, at the same add acetone suppress APP hydrolysis work
With, and by limiting the temperature and humidity of determination of the environment, the environmental requirement of measure had both been met, while it also avoid acetone volatilization
Fast and cuvette surface is hazed phenomenon so that measurement result deviation is improved using colorimetric method for determining aggregate rate within 5%
Accuracy, and it is preferable to test reappearance.
Embodiment：
S1：The preparation of standard liquid and Specification Curve of Increasing：
(1) first prepares phosphorus standard reserving solution：
The potassium dihydrogen phosphate of the 1.9157g drying two hours at 105 DEG C in advance is dissolved in water, is settled to 1L, this solution five
It is 1mg/ml to aoxidize two phosphorus concentrations；
(2) prepares phosphorus standard liquid with phosphorus standard reserving solution：The accurate phosphorus standard reserving solution pipetted in 10ml steps (1)
In 100ml volumetric flasks, 100ml is settled to, this solution is standard liquid, and the concentration of this solution is 0.1mg/ml.
(3) standard liquid 0ml, 5ml, 10ml, 15ml, 20ml of known phosphorus content are taken respectively into 50ml volumetric flasks, so
Addition 25ml, concentration 99.5% analyze pure acetone and carry out freezing 20 minutes afterwards, and then adding concentration in each volumetric flask again is
37.6mg/ml ammonium molybdate solution 4ml constant volumes, control indoor temperature in 20 DEG C or so, indoor relative humidity at 55 degree or so,
Absorbance is determined at 430nm.The absorbance of surveyed solution is determined using ultraviolet-uisible spectrophotometer, is then marked according to known
Relation automatic Fitting curve and fitting equation between the phosphorus content of quasi- solution and the absorbance for determining solution.
S2：2ml sample is weighed, then addition 1ml, concentration are 1mg/ml sodium hydroxides, stirring, make its pH value left 8
It is right.
S3：The mixture of above-mentioned steps is filtered, then takes 25ml acetone in 50ml volumetric flasks, after freezing 20min,
Addition concentration is 37.6mg/ml ammonium molybdate 4ml constant volumes, with constant volume after orthophosphates reaction generation complex compound, controls indoor temperature
In 20 DEG C, indoor relative humidity at 55 degree, then phosphorus content X2 is 14.2867% in orthophosphates in measure sample.
S4：Filtered after taking sample constant volumes of the 100mg-200mg in terms of phosphorus pentoxide, then take 25ml filtrates in 500ml
In beaker, add the heating of 10ml salpeter solutions and boil, be cooled to room temperature, take 2ml in 50ml volumetric flasks, it is cold to add acetone 25ml
After freezing 20min, addition concentration is 37.6mg/ml ammonium molybdate 4ml constant volumes, and control indoor temperature exists in 20 DEG C, indoor relative humidity
55 degree, the content X1 for being then measured phosphorus pentoxide in sample is 28.5946%；
S5：According to the data of phosphorus pentoxide content X1 in phosphorus content X2, water-soluble phosphorus in the orthophosphates of above-mentioned acquisition, press
Aggregate rate y is calculated according to equation below：
X1=28.5946%, X2=14.2867%
From above-mentioned result of calculation, the aggregate rate that method of testing of the present invention is obtained is used as 50.04%, it is known that it is poly-
Conjunction rate is 50%, and its deviation is within 5%.
Figure below is 4 samples of known aggregate rate, using the colorimetric method for determining aggregate rate of prior art and using the present invention
The correction data of colorimetric method for determining aggregate rate.
From above-mentioned correction data, the aggregate rate result determined using the present invention is more accurate, and deviation 5% with
It is interior.
In summary, it is only the part of present pre-ferred embodiments shown in the above embodiment of the present invention, can not be with this office
The limit present invention, under conditions of marrow of the present invention is not departed from, any modification that those skilled in the art are made, equivalent substitution and change
Enter, all belong to protection scope of the present invention.
Claims (7)
- A kind of 1. method of the quick measure aggregate rate of fertilizer sample containing APP, it is characterised in that comprise the steps：Standard curve is drawn according to the relation between the content and absorbance of standard substance；Adjust sample to be tested acid-base value；Determine phosphorus content in the orthophosphates in sample to be tested：A certain amount of acetone is added in sample to be tested, is added after freezing Constant volume, 10-20 DEG C of control indoor temperature and relative humidity 45-55 degree after ammonium molybdate, with orthophosphates reaction generation complex compound, so After be measured；Determine the content of water-soluble phosphorus in sample to be tested：Filtered after taking a certain amount of sample to be tested constant volume, take appropriate filtrate in burning In cup, add salpeter solution heating and boil, taken after cooling in right amount in volumetric flask, add acetone freezing, add ammonium molybdate constant volume, 10-20 DEG C of indoor temperature and relative humidity 45-55 degree are controlled, is then measured；According to the orthophosphates phosphorus content of above-mentioned acquisition, the data of water-soluble phosphorus content, aggregate rate y is calculated according to equation below：<mrow> <mi>y</mi> <mo>=</mo> <mfrac> <mrow> <mi>x</mi> <mn>1</mn> <mo>-</mo> <mi>x</mi> <mn>2</mn> </mrow> <mrow> <mi>x</mi> <mn>1</mn> </mrow> </mfrac> <mo>&times;</mo> <mn>100</mn> </mrow>In formula：X1---- sample reclaimed water soluble phosphorus contentsPhosphorus content in orthophosphates in X2----- samples.
- 2. the method for the quick measure aggregate rate of fertilizer sample containing APP as claimed in claim 1, it is characterised in that described The step of drawing standard curve is to draw standard liquid into 50m l volumetric flasks, adds acetone and freezes 20 minutes, adds 4m l Constant volume after ammonium molybdate solution, control indoor temperature less than 20 DEG C, indoor relative humidity below 55 degree, at 430nm measure Absorbance.
- 3. the method for the quick measure aggregate rate of fertilizer sample containing APP as claimed in claim 1, it is characterised in that select Inorganic base adjusts the sample to be tested acid-base value, and ph is between 7.5-8.5 for regulation.
- 4. the method for quick measure fertilizer sample containing the APP aggregate rate as described in claim any one of 1-3, its feature It is, in the orthophosphates in phosphorus detection step, the addition of the acetone is the 40%- of sample to be tested weight 60%.
- 5. the method for quick measure fertilizer sample containing the APP aggregate rate as described in claim any one of 1-3, its feature It is, in the orthophosphates in phosphorus detection step, the addition of the ammonium molybdate is the 5%- of sample to be tested weight 10%.
- 6. the method for quick measure fertilizer sample containing the APP aggregate rate as described in claim any one of 1-3, its feature It is, in the assay step of the water-soluble phosphorus, the salpeter solution concentration is 40%-60%.
- 7. the method for quick measure fertilizer sample containing the APP aggregate rate as described in claim any one of 1-3, its feature It is, in the assay step of the water-soluble phosphorus, the addition of the acetone is the 40%-60% of sample to be tested weight.
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| 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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| CN1991339A (en) * | 2005-12-30 | 2007-07-04 | 中国石油化工股份有限公司 | Method for analyzing total phosphorus content in sample |
| CN103698448A (en) * | 2013-12-05 | 2014-04-02 | 华南农业大学 | Method for fast separation and determination of phosphates in different forms in ammonium polyphosphate |
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| CN1991339A (en) * | 2005-12-30 | 2007-07-04 | 中国石油化工股份有限公司 | Method for analyzing total phosphorus content in sample |
| CN103698448A (en) * | 2013-12-05 | 2014-04-02 | 华南农业大学 | Method for fast separation and determination of phosphates in different forms in ammonium polyphosphate |
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