20.500.12556/DKUM-39322 DOLOČANJE VSEBNOSTI N,N' diizo propil etilen diamina S PLINSKO KROMATOGRAFIJO DETERMINATION OF N,N' diiso propyl ethylene diamine WITH GAS CHROMATOGRAPHY Namen diplomskega dela je bil dokazati, da je analizna metoda za določanje vsebnosti N,N' diizo propil etilen diamina (v nadaljevanju: Dipeda) s plinsko kromatografijo natančna, ponovljiva, točna, linearna v določenem območju, selektivna in robustna. Dipeda se uporablja za proizvodnjo antibiotikov, in sicer kalijevega klavulanata. Za določevanje vsebnosti smo uporabili plinsko kromatografijo s plamensko ionizacijskim (FID) detektorjem. Zaradi higroskopnosti Dipede smo analize izvedli z dodatkom internega standarda. Za kalibracijo sistema smo uporabili certificirani referenčni standard. Vse rezultate smo statistično ovrednotili s statističnimi testi, glede na zahteve validacijskega protokola. Z validacijo smo potrdili vse zahtevane validacijske kriterije . Pomemben del validacije je bil preizkus stabilnosti raztopin standardov in vzorcev. Ustrezna stabilnost je potrebna zaradi avtomatskih vzorčevalnikov in težnje po čim hitrejšem izvajanju analiz. Avtomatski vzorčevalnik omogoča izvajanje analize v eni sekvenci tudi več dni, zato moramo zagotoviti ustreznost raztopin vzorcev in standardov. The aim of this thesis is to demonstrate that the analytical method for the determination of N, N 'di-iso propyl ethylene di-amine (hereinafter Dipeda) by using gas chromatography is accurate, repeatable, exact, linear within a certain range, selective, and robust. Dipeda is used for the production of antibiotics, namely potassium clavulanate. To determine its content gas chromatography with flame ionization (FID) detectors was deployed. Because of Dipede hygroscopicity, the analysis was performed by taking into account an internal standard. For calibration of the system, a certified reference standard was used. All results were statistically evaluated using statistical tests with regard to the requirements of validation protocols. All the required validation criteria were confirmed in the validation process. An important part of the validation was to test the stability of solutions of standards and samples. Adequate stability is necessary because of automatic samplers and the tendency of rapid analysis implementation. The autosampler allows for analysis in a sequence of several days, so appropriate solution samples and standards need to be ensured. N N' diizo propil etilen diamin Dipeda plinska kromatografija plamensko ionizacijski detektor napake v analizni kemiji validacija UDK: 543.544.3.054(043.2) N N' di-iso propyl ethylene di-amine Dipeda gas chromatography flame ionization detector errors in analytical chemistry validation true true false [C. Kelenc] Slovenski jezik Angleški jezik Diplomsko delo 2012-12-28 16:59:34 2013-01-04 10:10:28 2022-05-04 14:21:00 2021-04-22 03:10:32 2012 0 Maribor 0 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 543.444.3.054(043.2) 16717334 URN:SI:UM:DK:TTWQIDTE VS_Kelenc_Cilka_2012.pdf VS_Kelenc_Cilka_2012.pdf 1 6CCB1384938FA301A7064795DE5BA09E 81a7cebf6621ebaaa975b587871a18d74d1c0047f9dca945d6e9d2315645dde9 1bbb0c2f-7c09-11eb-bb7a-00155d0001ca 20.500.12556/dkum/13c84db0-498f-4f8c-a65f-fd1461cf37ec https://dk.um.si/Dokument.php?lang=slv&id=53106 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0