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Title:Karakterizacija in uporaba optičnih senzorjev za on - line in in - situ merjenje plinov v biotehnoloških procesih
Authors:ID Brglez, Polonca (Author)
ID Kolar, Mitja (Mentor) More about this mentor... New window
Files:.pdf DR_Brglez_Polonca_2013.pdf (4,84 MB)
MD5: 8B4862F23355050DB4F861B8792C5CDD
 
Language:Slovenian
Work type:Dissertation
Typology:2.08 - Doctoral Dissertation
Organization:FKKT - Faculty of Chemistry and Chemical Engineering
Abstract:Doktorska disertacija je razdeljena na več sklopov, v katerih smo poskušali poglobiti dosedanje raziskave na področju optičnega senzorja kisika na osnovi 4,7 - difenil - 1,10 - fenantrolin rutenijevega(II) diklorid kompleksa - (Ru(dpp)3). Namen doktorskega dela je bila izboljšava optičnih lastnosti in odziva senzorjev na osnovi Ru(dpp)3. Lastnosti senzorja smo dodatno raziskali s poudarkom na preučevanju različnih tehnik izdelave senzorjev, spreminjanja koncentracij barvila, aplikacije različnih polimernih nosilcev, vpliva potencialnih interferenčnih plinov in vključevanja nanodelcev. Izdelali smo tankoslojne optične senzorje kisika s pomočjo različnih tehnik nanosa senzorskih raztopin (»spin coating« tehnike, s pomočjo naprave za tanke nanose in s pomočjo mehanskega nanosa). Namen je bil pripraviti najbolj homogen nanos senzorske raztopine in tako dobiti najbolj optimalne lastnosti senzorjev. Nanašanje senzorske raztopine s pomočjo mehanskega nanosa je enostavna in cenovno najbolj ugodna tehnika. Vendar se ta tehnika ni izkazala kot najprimernejša, saj je težko zagotoviti popolnoma homogen nanos po celotni senzorski površini. Ugotovili smo, da je glavna prednost uporabe »spin coating-a« ta, da je tehnika hitra, enostavna za uporabo in primerna za nanos majhnih volumnov. Omogoča izdelavo več serij senzorjev z različnimi lastnostmi ob minimalni porabi reagentov. »Spin coating« se je izkazal kot učinkovita metoda za nanos senzorskih raztopin v laboratorijskem merilu, vendar je po celotni senzorski površini težko pripraviti popolnoma homogen nanos (150 µL senzorske raztopine, 80 mg Ru(dpp)3, kloroform, silikon E41, folija Dataline, program na »Spin coater-ju«: 1. korak: 750 obr.  3 s, 2. korak: 300 obr.  3 s in 3. korak: 150 obr.  3 s). Kot najprimernejša tehnika za nanos senzorskih raztopin se je izkazala metoda nanosa senzorske raztopine s pomočjo naprave za tanke nanose, kjer smo nanašali senzorske raztopine v debelini: 10 µm, 15 µm, 20 µm, 25 µm, 30 µm, 40 µm in 50 µm. Ta način izdelave omogoča najbolj homogen nanos senzorske raztopine, postopek je hiter, enostaven in omogoča izdelavo večjih količin senzorjev s ponovljivimi lastnostmi. Ugotovili smo, da so se z dodajanjem različnih kovinskih nanodelcev in Triton - X, karakteristike senzorjev izboljšale. Pri uporabi senzorjev v realnih pogojih smo spremljali vsebnost kisika med postopkom biološke razgradnje, kjer imajo elektrokemijski senzorji omejitve. Elektrode iz plemenitih kovin, ki reagirajo s korozivnimi plini, zato niso primerne za tovrstne aplikacije. S pomočjo optičnega senzorja kisika na osnovi Ru(dpp)3 smo spremljali koncentracijo kisika pri razgradnji organskih odpadkov; le-ta je ključnega pomena pri proizvodnji komposta. Študirali smo tudi razgradnjo mešanih organskih odpadkov s pomočjo mikroorganizmov v avtomatskem kompostniku, ki je učinkovitejši način, v kolikor se odločimo za kompostiranje na domu. Za optimalno delovanje avtomatskega kompostnika so potrebne še dodatne študije, ki bodo vključevale drugačne pogoje kompostiranja (različne substrate in mešanice substratov, selekcionirane mikroorganizme, spremljanje nastanka plinov itd.). Tretjo uporabnost razvitega senzorja smo preizkusili na področju meritev sestave bioplina. Merjenja, ki se lahko izvajajo on-line ali in-situ nam lahko povedo bistveno več o samem procesu in tako dajejo možnost vplivanja ter optimizacije procesa nastanka bioplina. Z merjenjem koncentracije kisika v pilotnem bioreaktorju smo dokazali, da je optični senzor kisika primeren tudi za merjenje kisika v bioplinu. Senzor ima sledeče prednosti: je enostaven za uporabo in omogoča meritve v vodi ali v plinskih fazi, je eksplozijsko varen in z njim lahko izvajamo meritve v vrtinah, kjer je podtlak ali nadtlak.
Keywords:4, 7 - difenil-1, 10-fenantrolin rutenijev(II) diklorid kompleks, optični senzor kisika, spin coating, kisik, bioplin, interference, mešalna komora, kompost, mešanje plinov, nanodelci
Place of publishing:Maribor
Publisher:[P. Brglez]
Year of publishing:2013
PID:20.500.12556/DKUM-42894 New window
UDC:543.42:543.279:602.4(043.3)
COBISS.SI-ID:270618368 New window
NUK URN:URN:SI:UM:DK:ZRXAVT07
Publication date in DKUM:29.11.2013
Views:2495
Downloads:226
Metadata:XML RDF-CHPDL DC-XML DC-RDF
Categories:KTFMB - FKKT
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Secondary language

Language:English
Title:Characterization and use of optical sensors for the on - line and in - situ measurement of gases in biotechnological processes
Abstract:PhD thesis is divided in a complex of research cases in the field of oxygen optical sensor, based on 4,7 – diphenyl - 1, 10 - phenanthroline ruthenium(II) dichloride complex - (Ru(dpp)3). The purpose of PhD thesis is to improve optical features and response of a sensor based on Ru(dpp)3. Additional research of sensor features was carried out with an emphasis on various techniques of making sensors, modification of dye concentration, application of different polymeric supports, influence of the interference effect and an emphasis on implementation of nanoparticles. Afterwards, oxygen optical sensor was made, using different techniques of sensor solutions applications (»spin coating« technique, using device for a thin layer and mechanical application). The purpose of the abovementioned was to prepare the most homogeneous sensor solution in order to obtain the most optimal sensor features. Applying sensor solutions with mechanical application is simple and the most cost advantageous technique. However, this technique has not proven to be the most appropriate, because it is difficult to ensure a homogeneous coating over the entire sensor surface. We found out that the main advantage of spin-coating use is its velocity, simplicity and its suitability for application of smaller volumes. It also enables a production of various series of sensors with different features and minimal reagent use. The spin coating method has proved effective when applying sensor solutions in laboratories, but it does face a few difficulties when it comes to preparation of homogeneous coating (150 µL of sensor solution, 80 mg of Ru(dpp)3, chloroform, silicon E41, Dataline foil, spin coater programme set on: 1st step: 750 spins  3 s, 2nd step: 300 spins  3 s and 3rd step: 150 spins  3 s). The most suitable method of applying sensor solutions is device for thin layer where the thickness of sensor solutions amounts to 10 µm, 15 µm, 20 µm, 25 µm, 30 µm, 40 µm and 50 µm. Such manufacturing method enables the most homogeneous application of sensor solution; it is fast, simple and enables a composition of sensors with reproducible properties. By adding various metal nanoparticles and Triton - X - 100, characteristics of the sensors were improved. When using the sensors in existing conditions, the content of oxygen during biodegradation was observed. Electrochemical sensors have limits, (electrodes, consisting of noble metals which react with corrosive gases); therefore they are not suitable for such application. Afterwards, the concentration of oxygen in decomposition of organic waste was observed with an oxygen optical sensor based on Ru(dpp)3. Furthermore, decomposition of mixed organic waste with microorganisms in automatic compost bin was studied, which is the most effective method when making the compost at home. For optimal working of an automatic compost bin, further studies are needed, which will include different conditions, (various strata and blends of strata, a selection of microorganisms, monitoring the occurrence of gas, etc.). Applicability of the sensor we developed was tested in the field of biogas and its measurements. Measurements which can be carried out on-line or in-situ can tell us a little more about the process itself and as such give a chance to optimize the process of biogas production. The measurement of oxygen concentration in pilot bioreactor has proven that oxygen optical sensor is suitable for measurement of oxygen in biogas. The advantages of the sensor are the following: it is easy to use, enables measurements in water or in gas phase, is explosion proof and the measurements can be carried out in wells where negative and positive pressure is present.
Keywords:4, 7 - diphenyl - 1, 10 - phenanthroline ruthenium(II) dichloride complex, the optical oxygen sensor, spin coating, oxygen, biogas, interference, a mixing chamber, compost, gas mixing, nanoparticles


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