Razvoj i validacija kromatografske metode za određivanje ostatnih otapala u proizvodnom mulju

master's thesis

• Title (english): Development and validation of a chromatographic method for the determination of residual solvents in production sludge
• Author: Jelena Bošnjak
• Mentor: Sandra Babić (mentor)
• Committee member: Sandra Babić (predsjednik povjerenstva)
• Committee member: Dragana Mutavdžić Pavlović (član povjerenstva)
• Committee member: Irena Škorić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2022-09-12, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Oporaba je termin koji se često veže uz model kružnog gospodarstva pa tako tvrtka Premifab d.o.o. oporabljuje otpadna organska otapala različitih industrija s ciljem produljenja vrijednosti proizvoda. Oporaba se vrši šaržnom destilacijom nakon čega u destilatoru zaostaje mulj raznovrsnog kemijskog sastava koji ostaje neiskorišten i zbrinjava se o vlastitom trošku. S ciljem davanja vrijednosti proizvodnom mulju, potrebno je odrediti njegov kemijski sastav. Cilj ovog rada bio je razviti i validirati kromatografsku metodu za određivanje ostatnih organskih otapala u proizvodnom mulju koji nastaje šaržnom destilacijom otpadnih organskih otapala. Metoda je razvijana na plinskom kromatografu s FID detektorom i headspace uzorkovanjem. Nakon razvoja metode provedena je validacija kako bi se potvrdila prikladnost metode za njezinu namjenu. Rezultati validacije pokazali su da je metoda prikladna za određivanje metanola, etanola, acetona, izopropanola, metil-etil-ketona, etil-acetata, cikloheksana, izooktana i toluena u proizvodnom mulju. Za određivanje ostalih organskih otapala - metoksi-2-propanola, butanola, metil-izobutil-ketona, etoksi-2-propanola, butil-acetata, etilbenzena i izomera ksilena - potrebna je daljnja optimizacija metode. Nakon validacije, analiziran je realni uzorak proizvodnog mulja koji je dobiven destilacijom smjese otpadnih otapala metil-etil-ketona i etil-ace-tata porijeklom iz industrije proizvodnje fleksibilne ambalaže. Primjenom metode unutarnjeg standarda i relativnog faktora odgovora, kvantifikacija ispitivanog uzorka proizvodnog mulja uspješno je provedena.

Abstract (english)

Recovery is a term that is often associated with the circular economy model. It is implemented in the company Premifab Ltd. that recovers waste organic solvents from various industries with the aim of prolonging product value. Recovery is carried out by batch distillation, after which distillation sludge of various chemical composition remains unused what leads to its disposal at company’s own expense. To give value to distillation sludge, it is necessary to determine its chemical composition. The aim of this work was to develop and validate a chromatographic method for the determination of residual organic solvents in distillation sludge obtained by batch distillation of waste organic solvents. The method was developed on a gas chromatograph with an FID detector and headspace sampling. After the method was developed, validation was performed to confirm the suitability of the method for its purpose. The validation results showed that the method is suitable for the determination of methanol, ethanol, acetone, isopropanol, methyl-ethyl-ketone, ethyl-acetate, cyclohexane, isooctane, and toluene in distillation sludge. For the determination of other organic solvents, methoxy-2-propanol, butanol, methyl-isobutyl-ketone, ethoxy-2-propanol, butyl-acetate, ethylbenzene and xylene isomers, further optimization of the method is required. After validation, a real sample of distillation sludge obtained by distilling a mixture of waste solvents methyl-ethyl-ketone and ethyl-acetate originating from the flexible packaging industry was analyzed. By applying the method of internal standard and relative response factor, quantification of the examined sample of production sludge was successfully performed.

• Keywords: ostatna organska otapala; proizvodni mulj; plinska kromatografija; headspace; razvoj metode; validacija
• Keywords (english): residual organic solvents; production sludge; gas chromatography; headspace; development; validation
• Language: croatian
• URN:NBN: urn:nbn:hr:149:671781
• Study programme: Title: Applied Chemistry - Graduate study; specializations in: Environmental chemistry and green technologies, Advanced materials and technologies, Applied organic chemistry; Course: Applied organic chemistry; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra primijenjene kemije (magistar/magistra primijenjene kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access; Embargo expiration date: 2023-09-01
• Created on: 2023-03-19 16:38:50