Method for detecting monomethylene diurea and dimethylene triurea in urea formaldehyde fertilizer

A technology of monomethylene diurea and dimethylene triurea is applied in the field of detection of different component contents in urea-formaldehyde fertilizers, which can solve the problems of increased detection cost, poor repeatability, long time period, etc. The effect of reducing nitrogen loss, simple operation and short production cycle

Inactive Publication Date: 2019-04-16
沈阳中科新型肥料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The time period of the method is long, the repeatability is not good, and a large amount of energy is consumed, which not only causes the uncertainty of the experiment, but also increases the cost of detection.

Method used

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  • Method for detecting monomethylene diurea and dimethylene triurea in urea formaldehyde fertilizer
  • Method for detecting monomethylene diurea and dimethylene triurea in urea formaldehyde fertilizer
  • Method for detecting monomethylene diurea and dimethylene triurea in urea formaldehyde fertilizer

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Experimental program
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Effect test

Embodiment 1

[0023] Obtaining pure products of monomethylene diurea and dimethylene triurea:

[0024] Mix urea and paraformaldehyde as raw materials according to a mass ratio of 10:1, use 50mL of water as a solvent, reflux at 70°C for 10 minutes, rotary evaporate, and dry to obtain a mixture of diurea and ditriurea, and then use it several times 50ml of water was recrystallized and separated to obtain monomethylene diurea, and the remaining solution was rotary evaporated to obtain the target product of ditriurea, which was characterized by infrared spectroscopy and mass spectrometry (see attached figure 1 And attached figure 2 ), it can be seen from the infrared spectrum that 1650cm -1 The peak is the characteristic peak of the carbonyl structure of di-diurea and di-triurea, 3447-3331cm -1 and 1557cm -1 for NH 2 and NH characteristic peaks, m / z=155 is a methylene diurea (M + Na), m / z=205 is ditrisourea (M + H), so it can be concluded that the synthesized substances are indeed pure s...

Embodiment 2

[0029] Urea-formaldehyde fertilizer sample processing and testing methods are as follows:

[0030] Accurately weigh 0.5000g of sample 1, put it in a 100mL volumetric flask, prepare a standard solution with a mixture of methanol and water at a volume ratio of 9:1, and set the volume to the mark. Take 5 mL of the above-mentioned sample solution and place it in a centrifuge tube, and use a centrifuge to adjust the rotation speed to 4000 rpm for 15 min. Pass through a 0.45um filter membrane to form a solution to be tested after filter membrane pretreatment for liquid chromatography testing. Test conditions: organic mobile phase 90%, inorganic mobile phase 10%, organic mobile phase is methanol, inorganic phase is water, flow rate is set to 1.0mL / min, injection volume is set to 10uL, chromatographic column is selected as C18 chromatographic column, Column temperature 25°C, detection wavelength of UV detector: λ ex = 240nm. Chromatogram after detection (see attached Figure 4 ) c...

Embodiment 3

[0034] Column temperature is set as 40 ℃, and other conditions are the same as embodiment 2, and the result peak time slightly changes, and other is constant, the relative standard deviation of gained parallel sample<8%, the relative standard deviation<5% of repeatability test.

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Abstract

The invention relates to a method for detecting contents of different components in a urea formaldehyde fertilizer, in particular to a method for detecting monomethylene diurea and dimethylene triureain the urea formaldehyde fertilizer by using a high performance liquid chromatography technology of an ultraviolet detector. Methanol-water extracting solution upper sample in a to-be-detected urea formaldehyde fertilizer sample is subjected to liquid chromatography determination, and the monomethylene diurea and the dimethylene triurea in the to-be-detected urea formaldehyde fertilizer sample are qualitatively and / or quantitatively determined. The method provided by the invention is long in determination time period, poor in repeatability, and needs to consume a large amount of energy, so that the uncertainty of experiments is caused, and the detection cost is increased. In tens of years in the past, the detection of the urea formaldehyde fertilizer product is highly focused by researchers all the time. The invention discloses a novel detection method which has the advantages of simplicity in operation, short detection period, small error, greenness, environmental protection and thelike.

Description

technical field [0001] The invention relates to a method for detecting the contents of different components in urea-formaldehyde fertilizers, in particular to a method for detecting monomethylenediurea and dimethylenetriurea in urea-formaldehyde fertilizers by using high-performance liquid chromatography with an ultraviolet detector. Background technique [0002] Generally, urea-formaldehyde, also known as urea-formaldehyde fertilizer, was first produced by BASF in 1955 and was the first commercially produced slow-release nitrogen fertilizer. It is formed by the condensation of urea and formaldehyde, and is a white, odorless powder or granule. According to the different molar ratios of urea and formaldehyde, urea-formaldehyde fertilizers with different condensation degrees (release periods) can be made. At present, the detection of urea-formaldehyde fertilizer products is mainly through the testing of cold water insoluble nitrogen, hot water insoluble nitrogen, activity coe...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74G01N2030/027
Inventor 段文龙石元亮房娜娜李杰王玲莉
Owner 沈阳中科新型肥料有限公司
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