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High performance liquid chromatography analysis method of urea and its impurity carbamylurea, methylene biuret

A technology of high performance liquid chromatography and methylene diurea, which is applied in the field of high performance liquid chromatography analysis method, can solve the problems of time-consuming, high operation cost and high requirements for inspection personnel, and achieves low detection limit, high sensitivity and precision. Good results

Inactive Publication Date: 2011-01-12
刘忠发 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Spectrophotometric analysis of methylene biurea and biuret is time-consuming and labor-intensive, requiring high inspection personnel, high operating costs and low efficiency
For the analysis method of methylene biurea and biuret in urea products by high performance liquid chromatography, there is no relevant standard release and article report

Method used

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  • High performance liquid chromatography analysis method of urea and its impurity carbamylurea, methylene biuret
  • High performance liquid chromatography analysis method of urea and its impurity carbamylurea, methylene biuret
  • High performance liquid chromatography analysis method of urea and its impurity carbamylurea, methylene biuret

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] laboratory apparatus:

[0024] LC-10ATVP high performance liquid chromatography (Shimadzu, Japan);

[0025] SPD-10ATVP UV-Vis detector (Shimadzu, Japan);

[0026] Hangzhou Puhui Technology Co., Ltd. Sepu 3000P chromatography workstation;

[0027] Ultrasonic degasser (Shanghai Ultrasonic Co., Ltd.);

[0028] Filter: filter membrane pore size 0.45μm.

[0029] Chromatographic conditions:

[0030] Chromatographic column: 250mm×4.6mm(id) stainless steel column, built with Kromasil-5μm-C 18 filler;

[0031] The mobile phase composition volume ratio: methanol: water = 3: 97, wherein the water is desalted water, and boiled, methanol is analytically pure, the mobile phase is filtered with a 0.45 μm filter membrane and degassed with ultrasonic waves for 30 minutes before use;

[0032] Flow rate: 0.35Ml / min;

[0033] Column temperature: room temperature;

[0034] Detection wavelength: 210nm;

[0035] Injection volume: 6μl;

[0036] Internal standard: melamine.

[0037] ...

Embodiment 2

[0090] Chromatographic conditions:

[0091] Mobile phase composition volume ratio: methanol: water = 10:90;

[0092] Flow rate: 0.30Ml / min;

[0093] Column temperature: room temperature;

[0094] Detection wavelength: 215nm;

[0095] Injection volume: 5μl;

[0096] Internal standard: melamine.

[0097] All the other implementation modes are the same as the first embodiment.

[0098] (1). Methylene diurea linear relationship:

[0099] Using samples containing different concentrations of methylene diurea, the detection curve equation of methylene diurea is C / C i =-0.107551+4.34741×A / A i .

[0100] (2). Urea linear relationship

[0101] Prepare urea samples with different concentrations, and the curve equation of urea obtained by detection is C / C i =-16.0711+190.29×A / A i .

[0102] (3). Biuret linear relationship

[0103] Select biuret samples with different concentrations, and the curve equation of urea is C / C i =-0.00752131+7.53833×A / A i .

[0104] Pipette 6 μl ...

Embodiment 3

[0126] Chromatographic conditions:

[0127] Mobile phase composition volume ratio: methanol: water = 4: 96;

[0128] Flow rate: 0.38Ml / min;

[0129] Column temperature: room temperature;

[0130] Detection wavelength: 205nm;

[0131] Injection volume: 7μl;

[0132] Internal standard: melamine.

[0133] All the other implementation modes are the same as the first embodiment.

[0134] (1). Methylene diurea linear relationship:

[0135] Using samples containing different concentrations of methylene diurea, the detection curve equation of methylene diurea is C / C i =-0.107541+4.34744×A / A i 4.

[0136] (2). Urea linear relationship

[0137] Prepare urea samples with different concentrations, and the curve equation of urea obtained by detection is C / C i =-16.0711+190.32×A / A i .

[0138] (3). Biuret linear relationship

[0139] Select biuret samples with different concentrations, and the curve equation of urea is C / C i =-0.00752128+7.53817×A / A i .

[0140] Pipette 6 μl...

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Abstract

Warm methanol with water (3+97) is used for sample dissolution. Methanol with water (3+97) is used as mobile phase. A stainless steel column with Kromasil-5Mu m-C18 as filler and an ultraviolet detector are used. A reversed phase liquid chromatography separation is implemented on urea, methylene diurea and biuret in the sample. Melamine is used as an internal standard for internal standard quantification. The precision and the recovery of the method exceed GB2440-2001 test method requirements. The method has the advantages of simple operation method and high automation degree. And the method is a significant innovation for the products detection.

Description

(1) Technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to analyzing the content of amide products and their biuret and methylene diurea impurities by using a high-performance liquid chromatography analysis method. (2) Background technology [0002] The scientific name of urea is carbonamide, which is widely used in agricultural production as a basic fertilizer, and is also used as a raw material for melamine and fine chemicals; in the process of urea production, industrial formaldehyde is often added to increase the viscosity of the material due to the need for granulation. The reaction produces methylene diurea, and at the same time generates biuret at high temperature; urea containing methylene diurea exceeds the standard, which is extremely harmful to the production of melamine and causes quality reduction in the production of fine chemicals; urea containing biuret exceeding the standard will cause damage...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89
Inventor 刘忠发徐海伟
Owner 刘忠发