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A kind of high performance liquid phase detection method of hexaphenoxycyclotriphosphazene

A technology of hexaphenoxycyclotriphosphazene and high-performance liquid phase, which is applied in the field of analytical chemistry, can solve the problems of low separation of raw materials or impurities, cumbersome pretreatment steps, and difficult operation, etc. Appropriate peak time and good stability

Active Publication Date: 2022-05-03
JINAN TAIXING FINE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

P-hexaphenoxycyclotriphosphazene detection methods in the prior art have Fourier transform infrared spectroscopy, nuclear magnetic resonance, X-ray diffraction analysis, mass spectrometry, high performance liquid chromatography, thermogravimetric analysis, differential scanning calorimetry, etc., these methods There are only qualitative analysis or the pretreatment steps are cumbersome, difficult to operate, the separation degree of raw materials or impurities is not high, and the cost is high.

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  • A kind of high performance liquid phase detection method of hexaphenoxycyclotriphosphazene
  • A kind of high performance liquid phase detection method of hexaphenoxycyclotriphosphazene
  • A kind of high performance liquid phase detection method of hexaphenoxycyclotriphosphazene

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Embodiment 1 6

[0020] Embodiment 1 hexaphenoxy cyclotriphosphazene content determination test

[0021] The embodiment of the present invention provides a high-efficiency liquid phase detection method for hexaphenoxycyclotriphosphazene, comprising the following steps:

[0022] Hexaphenoxycyclotriphosphazene: produced by Shandong Taixing New Materials Co., Ltd.;

[0023] High performance liquid chromatography conditions:

[0024] Chromatographic column: WondaSil C18-WR, size 5μL, 4.6×150mm;

[0025] The mobile phase ratio is: a mixed solution of acetonitrile and methanol with a volume ratio of 50:10;

[0026] Use isocratic elution;

[0027] The detection wavelength is 210nm, the flow rate is 0.6mL / min, the column temperature is 27°C, the injection volume is 20μL, and the injection concentration of the sample solution is 0.1mg / mL.

[0028] Sample solution preparation: Accurately weigh about 10 mg of hexaphenoxycyclotriphosphazene into a 50 mL beaker, add an appropriate amount of acetonitril...

Embodiment 2 6

[0030] The precision test of embodiment 2 hexaphenoxy cyclotriphosphazene content determination

[0031] Hexaphenoxycyclotriphosphazene sample: 190824, produced by Shandong Taixing New Materials Co., Ltd.;

[0032] High performance liquid chromatography conditions:

[0033] Chromatographic column: WondaSil C18-WR, size 5μL, 4.6×150mm;

[0034] The mobile phase ratio is: a mixed solution of acetonitrile and methanol with a volume ratio of 50:10;

[0035] Use isocratic elution;

[0036] The detection wavelength is 210nm, the flow rate is 0.6mL / min, the column temperature is 27°C, the injection volume is 20μL, and the injection concentration of the sample solution is 0.1mg / mL.

[0037] Sample solution preparation: Accurately weigh 10.02 mg of hexaphenoxycyclotriphosphazene into a 50 mL beaker, add an appropriate amount of acetonitrile to dissolve, transfer to a 100 mL volumetric flask and dilute to the mark, and shake well. The concentration of this sample solution is 0.1002m...

Embodiment 3 6

[0041] The repeatability test of embodiment 3 hexaphenoxy cyclotriphosphazene content determination

[0042] Hexaphenoxycyclotriphosphazene sample: 1900808, produced by Shandong Taixing New Materials Co., Ltd.;

[0043] High performance liquid chromatography conditions:

[0044] Chromatographic column: Wondasil C18-WR, specification 5μL, 4.6×150mm;

[0045] The mobile phase ratio is: a mixed solution of acetonitrile and methanol with a volume ratio of 50:10;

[0046] Use isocratic elution;

[0047] The detection wavelength is 210nm, the flow rate is 0.6mL / min, the column temperature is 27°C, the injection volume is 20μL, and the injection concentration of the sample solution is 0.1mg / mL.

[0048] Sample solution preparation: Accurately weigh 6 parts of the same hexaphenoxycyclotriphosphazene sample (10.02mg, 10.06mg, 10.10mg, 10.03mg, 10.09mg, 10.13mg) into a 50mL beaker, add an appropriate amount of acetonitrile to dissolve, Transfer to a 100mL volumetric flask and dilute...

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Abstract

The invention discloses a high-efficiency liquid phase detection method for hexaphenoxycyclotriphosphazene. The sample solution containing hexaphenoxycyclotriphosphazene is passed into a chromatographic column, and the liquid phase chromatographic area normalization method is used for detection. Detection analysis. The detection method of the present invention has the characteristics of high accuracy and good stability; the separation between hexaphenoxycyclotriphosphazene and various raw material residues and impurities is relatively good, and the peak eluting time is relatively suitable. The method provided by the invention can better realize the determination of hexaphenoxycyclotriphosphazene, is beneficial to guide the control of raw materials and impurities in the production process, and obtain high-quality hexaphenoxycyclotriphosphazene.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a high-efficiency liquid phase detection method for hexaphenoxycyclotriphosphazene. Background technique [0002] Hexaphenoxycyclotriphosphazene is a cyclic phosphazene compound, which is light yellow or off-white powder or crystal, and is a widely used flame retardant. It is widely used in flame retardant fields such as polyethylene, fiber, yarn, fabric and copper clad laminate. The content of this product has a great influence on the flame retardant effect of the product. Therefore, it is necessary to detect and monitor hexaphenoxycyclotriphosphazene. P-hexaphenoxycyclotriphosphazene detection methods in the prior art have Fourier transform infrared spectroscopy, nuclear magnetic resonance, X-ray diffraction analysis, mass spectrometry, high performance liquid chromatography, thermogravimetric analysis, differential scanning calorimetry, etc., these methods Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 宋传君索伟李晶冯菲菲冯倩倩肖学文王艳辉
Owner JINAN TAIXING FINE CHEM