Визначення 2-бромоаніліну у вигляді триазену методом верх
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Date
2016
Authors
Мага, Іван
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Abstract
Встановлено оптимальні умови проведення реакції утворення триазену 2-бромоаніліну з 4-нітрофенілдіазоній катіоном: рН 5,5–7,5; 10–20-кратний надлишок реагенту. Лінійна залежність площі
хроматографічного піка від концентрації 2-бромоаніліну спостерігається в межах 20–5000 мкг/дм3.
Розроблено методику визначення 2-бромоаніліну в ґрунтах методом ВЕРХ. Методику апробовано на
модельних зразках та на реальному об’єкті. Проведено метрологічну обробку результатів.
Description
Triazine 2-bromoanilin (BA) has been synthesized. The synthesis was carried out in aqueous-ethanol
solution at p H5 (phosphate buffer solution) by azoderivation reactions with 4-nitrophenyl diazonium
cation. By elemental analysis, the structure of the resulting triazenes proved to contain carbon, chlorine,
hydrogen, and nitrogen.
Optimal conditions for the formation of triazenes BA were defined by the ionic form release, which
allows to eliminate the systems prevention impact. Azo compound BA occurs in a wide range of concentration
of hydrogen ions from pH 2 to pH 11, but the maximum yield of BA triazenes occurs within the pH of 4.5–7.
Reduction of the output of BA triazenes at pH < 4.5 is due to the dominance of the original amine form, and
decrease at pH > 7 by the decrease in the concentration of diazonium cations.
For extraction and removal of triazenes we investigated a number of organic solvents of different classes.
In particular: aliphatic hydrocarbons (hexane, heptane), aromatic hydrocarbons (benzene, toluene,
o-xylene); halogen derivatives of aliphatic hydrocarbons (dichloromethane, chloroform, dichloroethane);
acetic acidesters (ethyl acetate, butyl acetate, isoamyl acetate). The best extractant was chloroform.
The linear dependence of chromatographic peak area on the BA concentrations was observed in the
range of 20–5000 mg/l. Chromatography was conducted for the obtained extract. Retention time is 9.4 min.
There is a single symmetrical peak indicating the absence contaminants overlay that could interfere with
determination. In the chromatogram there is a significant peak of such impurities retention time of 7.4
minutes, which has a small area and does not overlap the peak of BA triazene. Maximum absorption of BA
triazene occurs at the end of the UV spectrum: at 388 nm. The kinetics and the impact on the number of
regent triazenes formation was studied. The experiment showed that azo derivate is formed quickly: within
1 minute. For complete reaction and maximum BA triazenes formation it is necessary to add 10–20 fold
excess of diazonium cations.
The study resulted in the method for determination of 2-chlorophenolesin soils by high performance
liquid chromatography. The method was tested on samples of the model and the real object.
Keywords
2-бромоанілін, триазен 2-бромоаніліну, реакція азодеривації, методика визначення, ВЕРХ
Citation
Мага Іван Михайлович. Визначення 2-бромоаніліну у вигляді триазену методом верх / Мага І. М. // Наукові записки НаУКМА. - 2016. - Т. 183 : Хімічні науки і технології. - С. 82-85.