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

Title of the article: Triphenylphosphine oxide interaction with zinc chloride in 2-butanol

Year: 2020, Issue: 6, Pages: 51-57

Branch of knowledge: 05.17.04 Technology of organic substances

Index UDK: 543.054

DOI: 10.26730/1999-4125-2020-6-51-57

Abstract: Preparation of samples with triphenylphosphine (TPP) when analyzing the products of oxidation of organic compounds by gas-liquid chromatography is carried out for quantitative conversion of compounds containing a hydroperoxide group into stable hydroxyl-containing derivatives. Triphenylphosphine reacts with hydroperoxide products contained in the sample and it is converted into triphenylphosphine oxide (TPPO). The triphenylphosphine oxide contained in the samples crystallizes in the discharge line and in the control valve and prevents the analysis by gas-liquid chromatography on capillary columns. It was proposed to remove TPPO from samples by making it react with zinc chloride to form complexes ZnCl₂ ((С₆Н₅)₃PO)₂ insoluble in most solvents according to a known reaction. Samples containing TPPO were treated with partially dehydrated zinc chloride. The quantitative determination of TPP and TPPO in the samples was carried out by gas-liquid chromatography on a packed stainless steel column 1000 x 3 mm in size with a 5% OV-17 silicone sorbent on an N-AW-super Chromatone, grain size 0.16-0.20 mm. The kinetics of TPPO interaction with zinc chloride in 2-butanol was studied at different initial TPPO: ZnCl₂ molar ratios of 1.0 - 3.0. It was shown that almost complete removal of TPPO from its solution in 2-butanol occurs in 18-24 hours at an initial molar ratio of ZnCl₂: TPPO = 3.0.

Key words: triphenylphosphine oxide zinc chloride 2-butanol sample preparation peroxide compounds gas-liquid chromatography

Receiving date: 10.12.2020

Publication date: 29.12.2020

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