CN101893554A - Method for quickly analyzing porous ammonium nitrate anticaking agent - Google Patents

Method for quickly analyzing porous ammonium nitrate anticaking agent Download PDF

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Publication number
CN101893554A
CN101893554A CN 201010217841 CN201010217841A CN101893554A CN 101893554 A CN101893554 A CN 101893554A CN 201010217841 CN201010217841 CN 201010217841 CN 201010217841 A CN201010217841 A CN 201010217841A CN 101893554 A CN101893554 A CN 101893554A
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anticaking agent
ammonium nitrate
standard solution
sample
porous ammonium
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CN101893554B (en
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沙淮丽
王仁宗
刘裕
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Hubei Fubang New Material Co., Ltd
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HUBEI FUBANG CHEMICAL SCIENCE-TECHNOLOGY Co Ltd
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Abstract

The invention relates to a method for quickly analyzing a porous ammonium nitrate anticaking agent. The method comprises the following steps of: determining an anticaking agent in porous ammonium nitrate by using spectrophotometry, namely, preparing standard solution and drawing a standard curve of a known anticaking agent; determining a computational formula according to the standard solution; and quickly analyzing the porous ammonium nitrate of an unknown anticaking agent by using the spectrophotometry under the same wavelength. The method for quickly analyzing the porous ammonium nitrate anticaking agent is used for analyzing the anticaking agent in the porous ammonium nitrate, chemical fertilizers and compound fertilizers. Compared with a frequently-used Soxhelt extraction method, the method has the advantages of simple operation, short analysis time, higher accuracy, low cost, simple and practical operation, low pollution and the like, and the method is easy to promote in fertilizer anticaking agent industry.

Description

A kind of method of quickly analyzing porous ammonium nitrate anticaking agent
Technical field
The present invention relates to a kind of method of quickly analyzing porous ammonium nitrate anticaking agent.
Background technology
Add anticaking agent in the multi-hole nitramines and can change granulation mechanism; and can effectively suppress the multi-hole nitramines caking; but the use cost of anticaking agent in order to control the consumption of anticaking agent, detects the content of anticaking agent in the multi-hole nitramines than higher with certain analytical approach in the production practices.Traditional porous ammonium nitrate anticaking agent analytical approach is to adopt the Soxhlet extraction process, and this ratio juris is: make organic solvent with isopropyl alcohol or phenixin, continue heating and the anticaking agent in the multi-hole nitramines was extracted in 6-8 hour under 70 ℃ of-80 ℃ of temperature.Extracting finishes the back and adopts vacuum evaporation 1.5-2 hour that organic solvent evaporation is complete, and last weighing grease is the quality of anticaking agent.This method exposes a lot of shortcomings, and at first the Soxhlet extracting generally needs 6-8 hour, and consuming time long, whole test is finished needs about 10 hours, can not instruct production fast.Whether the technology that adopts vacuum evaporation to remove in addition to desolvate is not really perfect, can not accurately judge organic solvent and remove totally, and it is bigger to take weighing method to calculate anticaking agent content error at last.The anticaking agent consumption of general multi-hole nitramines is at 800-1000ppm, and the error of analytical balance weighing is very big.Therefore the Soxhlet method for extracting exists: one, length consuming time, two, complex operation step, three, defective such as accuracy is low.
Summary of the invention
Purpose of the present invention provides the method for anticaking agent in a kind of quickly analyzing porous ammonium nitrate for defectives such as the length consuming time, inconvenient operation, the accuracy that overcome conventional Soxhlet extraction process and have are low.This method adopts spectrophotometric method can quick and precisely analyze the content of anticaking agent in the multi-hole nitramines, brings very big facility to production.
The present invention realizes in the following manner:.
A kind of method of quickly analyzing porous ammonium nitrate anticaking agent, mainly carry out according to following steps:
(1) testing sample preparation: accurately take by weighing 50g and contain the multi-hole nitramines sample dissolution of unknown quantity anticaking agent in 50ml isopropyl alcohol organic solvent;
(2) sample dissolution and filtration: the multi-hole nitramines sample after will dissolving is cooled to room temperature after placing 50 ℃ of constant temperature water baths to be incubated half an hour, then with sample filtering;
(3) anticaking agent standard solution preparation: accurately take by weighing the 0.025g anticaking agent, dissolve and be diluted to 250ml with a small amount of isopropyl alcohol, it is 0.01mg/ml that this standard solution contains anticaking agent;
(4) typical curve is drawn: measure 0.0,1.0,2.0,4.0,6.0,8.0ml anticaking agent standard solution places 100ml volumetric flask and constant volume respectively, preparation massfraction 0.00,100ppm, 200ppm, 400ppm, 600ppm, the series standard solution of 800ppm is measured the absorbance of each standard solution under the 308nm wavelength, make the typical curve of this anticaking agent, and to try to achieve computing formula be Y=Kx+b; Wherein x is an absorbance, and Y is the anticaking agent amount;
(5) testing sample analysis: the testing sample solution after step (2) filtration is analyzed its absorbance A under the wavelength of 308nm, try to achieve the anticaking agent amount according to the computing formula of step (4).
The method of anticaking agent content is in the quickly analyzing porous ammonium nitrate provided by the invention: comprise The pretreatment and heating for dissolving, measure the absorbance of each standard solution under suitable wavelength, make the typical curve of this anticaking agent, obtain the computing formula several steps.
The present invention can be used for the analysis of multi-hole nitramines, composite fertilizer or artificial fertilizer anticaking agent.
The present invention compared with prior art, its advantage mainly comprises:
One, shorten analysis time, traditional Soxhlet extracting needs about 10 hours, and the about 1h-1.5h of present analytical approach has shortened analysis time greatly.
Two, operation steps is simple, and traditional method needs a plurality of steps such as Soxhlet extracting, vacuum evaporation, constant weighing, only needs sample preparation and spectrophotometer analysis now, easy operating.
Three, accuracy height, traditional method running time is long, complex steps, source of error is extensive, and present analytical approach adopts spectrophotometric method sensitivity very high, can be used in a small amount of and micro-example analysis.
Embodiment
The invention will be further described below in conjunction with embodiment.
A kind of method of quickly analyzing porous ammonium nitrate anticaking agent, carry out according to following steps:
(1) testing sample preparation: the multi-hole nitramines sample dissolution that contains anticaking agent that takes by weighing article number that 50.012g buys from flower king (Shanghai) trade Co., Ltd and be FA80N is 50g isopropyl alcohol organic solvent;
(2) sample dissolution and filtration: the multi-hole nitramines sample after will dissolving places 50 ℃ of constant temperature water baths to be cooled to room temperature after half an hour, then with sample filtering;
(3) typical curve is drawn: measure 0.0,1.0,2.0,4.0,6.0,8.0ml anticaking agent standard solution places 100ml volumetric flask and constant volume respectively, preparation massfraction 0.00,100ppm, 200ppm, 400ppm, 600ppm, the series standard solution of 800ppm, the absorbance of measuring each standard solution under the 308nm wavelength is as follows:
Concentration (ppm) 0 100 200 400 600 800
Absorbance (A) 0 0.074 0.126 0.253 0.378 0.506
Make the typical curve of this anticaking agent, and to try to achieve computing formula be Y=1.6018x-0.0053, R2=0.9995 (degree of confidence of this formula is higher); Wherein x is an absorbance, and Y is the anticaking agent amount;
(4) testing sample analysis: the testing sample solution after step (2) filtration is analyzed its absorbance A under the wavelength of 308nm be 0.458, and according to computing formula Y=1.6018x-0.0053, trying to achieve the anticaking agent amount is 728ppm.
In order to verify property quick and precisely of the present invention, now adopt the multi-hole nitramines of two kinds of known anti-caking agent contents: its anti-caking agent addition is respectively 1000ppm, and 800ppm carries out the contrast test of two kinds of methods, and the result is as follows:
Figure BSA00000176077500031
From analytical table as can be seen: the anti-caking agent content of taking conventional Soxhlet method for extracting to analyze is low than standard sample, and the error between the parallel sample is also very big.Methods analyst resultant error of the present invention is little, and the error between the parallel sample is also all in the permissible error scope.

Claims (1)

1. the method for a quickly analyzing porous ammonium nitrate anticaking agent is carried out according to following steps: (1) testing sample preparation: accurately take by weighing 50g and contain the multi-hole nitramines sample dissolution of unknown quantity anticaking agent in 50g isopropyl alcohol organic solvent;
(2) sample dissolution and filtration: the multi-hole nitramines sample after will dissolving places 50 ℃ of constant temperature water baths to be cooled to room temperature after half an hour, then with sample filtering;
(3) anticaking agent standard solution preparation: accurately take by weighing the 0.025g anticaking agent, dissolve and be diluted to 250ml with a small amount of isopropyl alcohol, it is 0.01mg/ml that this standard solution contains anticaking agent;
(4) typical curve is drawn: measure 0.0,1.0,2.0,4.0,6.0,8.0ml anticaking agent standard solution places 100ml volumetric flask and constant volume respectively, under the 308nm wavelength, measure the absorbance of each standard solution, make the typical curve of this anticaking agent, and to try to achieve computing formula be Y=Kx+b; Wherein x is an absorbance, and Y is the anticaking agent amount;
(5) testing sample analysis: the testing sample solution after step (2) filtration is analyzed its absorbance A under the wavelength of 308nm, try to achieve the anticaking agent amount according to the computing formula of step (4).
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102243181A (en) * 2011-04-08 2011-11-16 湖北富邦科技股份有限公司 Method for detecting ammonia value of powdered anticaking agent
CN104237046A (en) * 2014-08-20 2014-12-24 湖北富邦科技股份有限公司 Method for rapidly measuring content of grease in chemical fertilizer
CN107831129A (en) * 2017-10-26 2018-03-23 天脊煤化工集团股份有限公司 Utilize the method for oil-like anti-caking agent content in spectrophotometry complex fertilizer

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1525949A (en) * 2001-06-12 2004-09-01 KAO�ɷ����޹�˾ Additives preventing caking and humectation of nitrogenous fertilizers
CN101522295A (en) * 2006-08-02 2009-09-02 奥姆尼亚肥料有限公司 Ammonium nitrate granules

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1525949A (en) * 2001-06-12 2004-09-01 KAO�ɷ����޹�˾ Additives preventing caking and humectation of nitrogenous fertilizers
CN101522295A (en) * 2006-08-02 2009-09-02 奥姆尼亚肥料有限公司 Ammonium nitrate granules

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《无机盐工业》 20040531 许瑞光 高氯酸钾晶体防结块技术研究及应用 24 1 第36卷, 第3期 2 *
《现代化工》 19981231 白树林 硝酸铵的防结块剂 43-44 1 , 第1期 2 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102243181A (en) * 2011-04-08 2011-11-16 湖北富邦科技股份有限公司 Method for detecting ammonia value of powdered anticaking agent
CN104237046A (en) * 2014-08-20 2014-12-24 湖北富邦科技股份有限公司 Method for rapidly measuring content of grease in chemical fertilizer
CN107831129A (en) * 2017-10-26 2018-03-23 天脊煤化工集团股份有限公司 Utilize the method for oil-like anti-caking agent content in spectrophotometry complex fertilizer

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Patentee before: Hubei Forbon Technology Co., Ltd.