20.500.12556/DKUM-39876 VALIDACIJA POSTOPKA DOLOČITVE MASNEGA DELEŽA KALCIJA V VZORCIH APNENČEVE MOKE IN OVREDNOTENJE MERILNE NEGOTOVOSTI REZULTATA DOLOČITVE KALCIJA VALIDATION AND MEASUREMENT UNCERTAINTY FOR DETERMINATION OF MASS FRACTION OF CALCIUM IN CALCITE SAMPLES Namen diplomske naloge je bil razviti in validirati kompleksometrično metodo za določanje masnega deleža kalcija v vzorcih apnenčeve moke z avtomatskim titratorjem in fotometrično določitvijo končne točke s fototrodo. V prvi stopnji razvoja preskusne metode smo pregledali obstoječo literaturo, priskrbeli referenčni material in kemikalije ter pripravili ustrezne raztopine. Z upoštevanjem optimalnih pogojev delovanja fototrode in z definiranjem titracijskih parametrov smo na avtomatskem titratorju izdelali dve kompleksometrični metodi: metodo za standardizacijo titracijske raztopine EDTA in metodo za določanje masnega deleža kalcija v vzorcih apnenčeve moke. Po izbiri ustreznih parametrov validacijskega postopka preskusne metode smo izvedli eksperimente, potrdili njeno primernost za predvideno uporabo in ovrednotili merilno negotovost rezultata določitve kalcija. Ugotovili smo, da je postopek določitve masnega deleža kalcija v vzorcih apnenčeve moke primeren za predvideno uporabo. Z validacijo smo dokazali, da je preskusna metoda natančna, točna, linearna in selektivna. Z ovrednotenjem merilne negotovosti rezultata določitve kalcija smo določili kakovost in lažjo primerljivost rezultatov. The purpose of this diploma thesis was to develop and validate a complexometric method for determination of the mass fraction of calcium in calcite samples using an automatic titrator and a photometric endpoint detection using a phototrode. During the initial phase of test method development the existing literature data was explored. The acquired reference materials and chemicals, as well as the preparation of the appropriate solutions were selected. Taking into account the optimal operating conditions of the phototrode and by defining the titration parameters, two complexometric methods using the titrator have been developed; namely the standardization of titrant EDTA method and the determination of the mass fraction of calcium in calcite samples method. After choosing the adequate characteristics of the test method validation procedure the experiments were conducted, which confirmed the suitability of the proposed method for its intended use. Measurement uncertainty of the results of calcium determination was evaluated. We established that the process for determination of mass fraction of calcium in calcite samples is suitable for its intended use. We have shown, through validation, that the test method is precise and accurate, as well as linear and selective. By evaluating the measurement uncertainty of the result of calcium determination the quality and easier comparability of the result have been established. kalcij kalcijev karbonat apnenčeva moka fotometrična določitev fototroda kompleksometrična titracija končna točka EDTA calcium calcium carbonate calcite photometric determination phototrode complexometric titration endpoint EDTA true true false [J. Ojsteršek] Slovenski jezik Angleški jezik Diplomsko delo 2013-03-12 14:17:12 2013-04-03 08:27:00 2022-05-12 23:16:38 2021-04-22 03:37:45 2013 0 Maribor 0 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 543.245:[666.364:553.55](043.2) 17461526 URN:SI:UM:DK:9OQCSYJZ VS_Ojstersek_Janja_2013.pdf VS_Ojstersek_Janja_2013.pdf 1 FC83BF267BA5498A9BE872DAD013C7A3 78b515aa1929ed8eb07b182d7bc6b7a309aa67e54839221d7e39c47158a33752 39b1ac54-7c09-11eb-bb7a-00155d0001ca 20.500.12556/dkum/31e03e34-0cdb-49f8-82c4-1219aec0de66 https://dk.um.si/Dokument.php?lang=slv&id=54220 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0