Določanje 1-hidroksicikloheksil fenil ketona in soli triarilsulfonijevega heksafluoroantimonata v polimernih materialih

Blatnik, Tjaša (author), Kralj Cigić, Irena (mentor)

Fotoiniciatorji so ključne spojine pri polimerizacijskih reakcijah. Pod vplivom svetlobe razpadejo na proste radikale, katione ali anione, ki sodelujejo pri polimerizacijskem procesu. Fotokatalizirane procese široko uporabljajo v tiskarstvu (UV-črnila, tisk na embalažne materiale, 3D tiskanje), medicini, sintezi polimernih materialov itd., saj imajo precej prednosti, kot so nizke emisije hlapnih organskih spojin (pomembno za okolje), prostorski in časovni nadzor (pomembno pri proizvodnji) in nizka poraba energije (ekonomski razlogi). Njihov vpliv na zdravje ljudi in razgradnjo izdelkov je v običajnih razmerah počasen in težko opazen proces, vendar je kumulativen, zato je pomembno poznavanje vsebnosti teh spojin. V magistrski nalogi sem se osredotočila na določanje fotoiniciatorjev, 1-hidroksicikloheksil fenil ketona (1-HCHPK) in soli triarilsulfonijevega tetrafluoroantimonata (THS), v vzorcih izbranih polimernih materialov. Identifikacijo in kvantifikacijo le-teh sem izvedla s pomočjo gradientne elucije s tekočinskim kromatografom v povezavi z detektorjem na niz diod, ki omogoča identifikacijo spojin na osnovi UV spektrov. S pomočjo pripravljenih umeritvenih krivulj sem določila vsebnost izbranih fotoiniciatorjev v vzorcih polimernih materialov. Določila sem tudi meje določitve in meje zaznave ter spremljala stabilnost fotoiniciatorjev, tako v raztopinah vzorcev kot tudi v standardnih raztopinah. Optimizirala sem ekstrakcijo spojin 1-HCHPK in THS iz polimernih materialov. Preverila sem, kako na učinkovitost ekstrakcije vpliva velikost delcev vzorca in sestava ekstrakcijskega topila. Ekstrakcijo sem izvedla z mešanico 0,1 % TFA in ACN v razmerju 7:3, tako da sem pripravljeno suspenzijo vzorca v ekstrakcijskem topilu postavila v sušilnik, segret na 70 °C za 21 h. Dobljeno raztopino sem filtrirala skozi 0,45 µm filter in nato injicirala v tekočinski kromatograf. Optimizirana metoda nam da ponovljive rezultate. Iz dobljenih rezultatov lahko povzamem, da velikost delcev vzorca vpliva na učinkovitost ekstrakcije, in sicer manjši kot so delci, bolj je ekstrakcija učinkovita, medtem ko sestava ekstrakcijskega topila ne vpliva na učinkovitost ekstrakcije. Na osnovi rezultatov analiz realnih vzorcev lahko zaključim, da vzorci niso homogeni in da se določevane spojine s časom razgrajujejo.

• Language: Slovenian
• Keywords: fotoiniciatorji, tekočinska kromatografija, polimerni materiali
• Work type: Master's thesis/paper
• Typology: 2.09 - Master's Thesis
• Organization: FKKT - Faculty of Chemistry and Chemical Technology
• Year: 2019
• PID: 20.500.12556/RUL-112593
• COBISS.SI-ID: 1538479811
• Publication date in RUL: 25.10.2019

Secondary language

• Language: English
• Title: Determination of 1-hydroxycyclohexyl phenyl ketone and salts of triarylsulfonium hexafluoroantimonate in polymeric materials

Abstract

Photoinitiators are the key compounds in polymeric reactions. Under the light they decompose to free radicals, cations, or anions which are part of polymerization process. Photoinitiators are widely used in printing (UV-inks, packaging materials print, 3D print), medicine, synthesis of polymeric materials etc. Photoinitiators have many advantages such as low emissions of volatile organic compounds (important for environment), area and time control (important with production) and low energy consumption (economy reasons). Their impact on human health and degradation of products is a slow and hardly noticeable process at usual conditions, but it is cumulative and therefore it is important to know the content of these compounds. In my master thesis I have focused on the determination of photoinitiators, 1-hydroxycyclohexyl phenyl ketone (1-HCHPK) and salts of triarylsulfonium hexafluoroantimonate (THS) in the samples of selected polymeric materials. Identification and quantification of photoinitiators was accomplished by using liquid chromatography with gradient elution. The diode array detector enabled the identification based on the UV spectra. On the basis of prepared calibration curves, I have determined the content of selected photoinitiators in the samples of polymeric materials. In addition, limit of detection and limit of quantification was determined in sample solutions as well as in the standard solution. I have optimized the extraction of compounds 1-HCHPK and THS from the polymeric materials. I have examined the influence of particle size of sample and composition of extraction solvent on the extraction efficiency. For the extraction a mixture of 0.1°% TFA and ACN in ratio 7:3 was used. The prepared suspension of sample in extraction solvent was in the dryer at the temperature of 70 °C for 21 h. Solution was than filtered through 0.45 µm filter and injected into liquid chromatograph. The optimized method gave repeatable results. To summarize the obtained results, particle size does influence the efficiency of the extraction. If the particles are smaller, the efficiency of the extraction is higher. Meanwhile the composition of extraction solvent does not influence the efficiency of the extraction. Based on the results of analyses of real samples, it can be concluded that the samples are not homogeneous and that determined compounds degrade over time.

• Keywords: photoinitiatiors, liquid chromatography, polymeric materials