Atomic absorption spectrometry of content of Fe and Zn impurities in yellow phosphorus

A technology of impurity content and determination method, applied in the direction of color/spectral characteristic measurement, test sample preparation, etc., can solve the problem of inability to directly measure Fe and Zn impurities in high-purity yellow phosphorus, and achieve precision and detection limit Satisfy, eliminate inhibitory effects

Inactive Publication Date: 2010-02-17
SICHUAN UNIV
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Problems solved by technology

[0005] In view of the present situation of iron and zinc impurity measurement technology in yellow phosphorus, the purpose of the present invention is to provide a new method for measuring Fe and Zn impurities in yellow phosphorus by atomic absorption spectrometry, so as to solve the problem that atomic absorption spectrometry cannot directly measure high-purity yellow phosphorus. Problems such as Fe and Zn impurities in medium, enrich the determination method of Fe and Zn impurities in yellow phosphorus

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  • Atomic absorption spectrometry of content of Fe and Zn impurities in yellow phosphorus
  • Atomic absorption spectrometry of content of Fe and Zn impurities in yellow phosphorus
  • Atomic absorption spectrometry of content of Fe and Zn impurities in yellow phosphorus

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Embodiment

[0023] 1. Determination of iron and zinc impurities

[0024] (1) the yellow phosphorus sample of iron-zinc impurity content to be measured is digested with the nitric acid of volume concentration 70%, and the sample solution that the phosphoric acid concentration is obtained is 0.6mol / l;

[0025] (2) Phosphoric acid in the sample solution prepared in step (1) is extracted and separated with tributyl phosphate, the volume ratio of the sample solution and tributyl phosphate is controlled to be 1: 1, and the extraction process time is about 10min, so that the sample solution About 80% (mol concentration) of the phosphoric acid in the solution is extracted, the organic phase is discarded, the water phase is retained, and the water phase is left to stand for about 30 minutes. The water phase after standing is the sample water used to measure zinc and iron impurities in yellow phosphorus phase solution, the treated sample water phase solution was constant volume, and set aside;

[...

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Abstract

The invention discloses an atomic absorption spectrometry of the content of Fe and Zn impurities in yellow phosphorus. The atomic absorption spectrometry mainly comprises the following steps: (1) heating and digesting yellow phosphorus by nitric acid with a volume concentration no lower than 50 percent to prepare a sample solution with a phosphoric acid concentration of 0.5-0.8mol/l; (2) extracting and separating phosphoric acid in the sample solution prepared in the step (1) by tri-butyl-phosphate, discarding organic phases and reserving a sample aqueous solution; (3) preparing a standard solution with different set concentrations of Fe and Zn, extracting the standard solution according to the same extracting condition of the step (2), measuring Fe and Zn of the obtained standard water-phase solution by a flame atomic absorption spectrometry method and drawing a working curve; (4) measuring the Fe and Zn of the sample water-phase solution obtained in the step (2) by the flame atomicabsorption spectrometry method and comparing a measurement result with the standard working curve measured and drawn in the step (3) to solve the content of Fe and Zn impurities in the yellow phosphorus sample to be measured.

Description

technical field [0001] The invention relates to a measurement technology of yellow phosphorus impurities, and more specifically relates to a method for measuring the content of iron and zinc impurities in yellow phosphorus. Background technique [0002] Yellow phosphorus is also called white phosphorus. Pure white phosphorus is a white waxy solid with a glossy appearance. Under the action of light and heat, it quickly turns yellow, so it is often called yellow phosphorus. Pure yellow phosphorus is odorless, but because it reacts with oxygen in the air to form ozone and phosphorus compounds, it often has a garlic-like odor. Yellow phosphorus is poorly soluble in water, slightly soluble in alcohol, easily soluble in phosphorus halogen compounds and carbon disulfide, and has certain solubility in benzene, toluene, ether and chloroform. Yellow phosphorus is active, and most elements can directly combine with it except carbon, boron, and silicon. Yellow phosphorus is highly pro...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N1/28G01N1/34
Inventor 朱晓帆钟本和许凤兰陈明柱李佳
Owner SICHUAN UNIV
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