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A kind of assay method of iron content in 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide

A determination method, the technology of phosphophenanthrene, which is applied in the direction of color/spectral characteristic measurement, etc., to achieve the effect of improved safety factor, less interference, and reduced operation process

Active Publication Date: 2017-10-27
湖北省兴发磷化工研究院有限公司
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Problems solved by technology

However, methods for detecting metal impurities in organic substances such as DOPO products, such as iron ions, have not been reported in Chinese literature

Method used

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  • A kind of assay method of iron content in 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide
  • A kind of assay method of iron content in 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide
  • A kind of assay method of iron content in 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide

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Experimental program
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Effect test

Embodiment 1

[0015] Testing conditions: TAS-986 Beijing General Analysis Atomic Absorption Spectrophotometer, flame method, air-acetylene flame, air outlet pressure 0.24Mpa, acetylene cylinder outlet pressure 0.05Mpa, acetylene flow rate 1400mL / min, wavelength 248.3nm, spectral bandwidth 0.2nm, lamp current 4.0mA, burner height 10mm. The filter coefficient is 0.6, and the integration time is 3 seconds. Use deuterium lamp buckle background.

[0016] Sample preparation: Weigh 1g (accurate to 0.1mg) sample, dissolve the sample with 50mL ethanol and quantitatively transfer it to a 100mL volumetric flask, add 2ml hydrochloric acid, shake well, then dilute to volume with secondary water, and prepare a blank solution at the same time. Select 5# sample and prepare 8 parallel samples.

[0017] Experiment: Pipette 0.00mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (40ug iron standard / mL) into 100mL volumetric flask, add 50mL ethanol, 2ml hydrochloric acid (GR), Make up...

Embodiment 2

[0021] Detection conditions: TAS-986 Beijing General Analysis Atomic Absorption Spectrophotometer, flame method, air-acetylene flame, air outlet pressure 0.24Mpa, acetylene cylinder outlet pressure 0.05Mpa, 1400mL / min, wavelength 248.3nm, spectral bandwidth 0.2nm , lamp current 4.0mA, burner height 10mm. The filter coefficient is 0.6, and the integration time is 3 seconds. Use deuterium lamp buckle background.

[0022] Linear equation experiment: pipette 0.00mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (50ug iron standard / mL) into 100mL volumetric flask, add 50mL ethanol, 2ml hydrochloric acid (GR ), and dilute to volume with secondary water. The absorbance value was measured under the same conditions. Perform linear regression on the iron ion concentration C with the absorbance value A of the solution, the regression equation is A=0.0644C+0.0066, and the correlation coefficient R=0.9976 (n=7).

[0023] Sample preparation: Weigh 1g (accurate t...

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Abstract

The invention relates to a method for measuring iron content in 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short), specifically by flame atomic absorption spectrophotometry. First prepare a sample solution with an appropriate concentration, vaporize the sample to be tested by a flame atomizer, and measure the content of the measured element iron in the sample based on the measurement of the absorption of the gaseous ground state atoms of the measured element iron to characteristic wavelength light . Compared with phenanthroline spectrophotometry, EDTA titration, ICP-OES, ICP-MS, flame atomic absorption spectrophotometry and other methods, it does not need to digest the sample, the safety factor is greatly improved, and the interference Small size, less reagents used, simple preparation, simple, fast and safe operation, low detection cost, good reproducibility and accuracy of detection results.

Description

technical field [0001] The invention relates to a method for determining the content of iron ions, in particular to a method for determining the content of iron ions in organic phosphorus heterocyclic compounds. Background technique [0002] DOPO is an organic phosphorus heterocyclic compound with high thermal stability, oxidation resistance and excellent water resistance. It is a reactive and additive flame retardant. [0003] Since the raw materials with iron ions are used in the synthesis of DOPO, the finished product of DOPO contains a certain amount of iron ions. In order to ensure the requirements of product quality, it is necessary to detect the iron ion content in DOPO. [0004] At present, there are many detection methods for iron ion content, such as o-phenanthroline spectrophotometry, EDTA titration, ICP-OES, ICP-MS, flame atomic absorption spectrophotometry and other methods. However, methods for detecting metal impurities in organic matter such as DOPO product...

Claims

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Application Information

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IPC IPC(8): G01N21/31
Inventor 李琴彭仁文郑群珍杜建侠盛美娥郝晓斌
Owner 湖北省兴发磷化工研究院有限公司
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