Authors: S.V. Puchkov, Yu.V. Nepomnyashchikh

Title of the article: Polypropylene compositions with reduced flammability

Year: 2021, Issue: 2, Pages: 40-46

Branch of knowledge: 05.17.04 Technology of organic substances

Index UDK: 544.144.7+547.264

DOI: 10.26730/1999-4125-2021-2-40-46

Abstract: Triphenylphosphinoxide (TFFO) formed during the treatment of samples containing hydrop-eroxide oxidation products of 2-butanol with triphenylphosphine prevents the analysis by gas-liquid chromatography (HPLC) on capillary columns. It has been shown that when TFFO is removed by treating samples with zinc chloride, the determined compounds react with the ZnCl2 to form complex compounds, and in the chromatograph evaporator during GLC analy-sis they undergo zinc chloride catalyzed transformations. These reactions distort the results of quantification of the products to be analyzed. To eliminate the distorting effect of the reac-tions of the determined products with zinc chloride during sample processing and during GLC analysis, a sample preparation technique was developed aimed at destroying the complex compounds of the determined products with zinc chloride and removing ZnCl₂ from the sam-ples. Proposed method of sample preparation consists in sequential treatment of samples with solid TFF for 20 min in 10% molar excess to total content of hydroperoxide products, fol-lowed by treatment with zinc chloride taken in three times molar excess to TFF for 24 hours. After separation of the resulting insoluble ZnCl₂ complex precipitate with TFFO, the samples were sequentially bubbled with hydrogen sulfide in the presence of acetic acid and sodium acetate. The resulting zinc sulfide precipitate was removed and the sample was held over po-tassium sulfide for 24 hours to remove traces of zinc. Zinc ion content was monitored by complexometric titration. The samples were concentrated in vacuo and then GLC analysis was performed.

Key words: triphenylphosphine oxide zinc chloride hydrogen sulfide potassium sulfide peroxide com-pounds gas-liquid chromatography

Receiving date: 06.03.2021

Publication date: 29.04.2021

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