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[{"key": "dc.contributor.author", "value": "Harju, Mauno", "language": null, "element": "contributor", "qualifier": "author", "schema": "dc"}, {"key": "dc.date.accessioned", "value": "2017-06-20T09:59:37Z", "language": "", "element": "date", "qualifier": "accessioned", "schema": "dc"}, {"key": "dc.date.available", "value": "2017-06-20T09:59:37Z", "language": "", "element": "date", "qualifier": "available", "schema": "dc"}, {"key": "dc.date.issued", "value": "1990", "language": null, "element": "date", "qualifier": "issued", "schema": "dc"}, {"key": "dc.identifier.uri", "value": "https://jyx.jyu.fi/handle/123456789/54598", "language": "", "element": "identifier", "qualifier": "uri", "schema": "dc"}, {"key": "dc.description.abstract", "value": "Ty\u00f6 jakautuu laajahkoon kirjalliseen osaan ja kokeelliseen osaan. Kirjallinen osa k\u00e4sittelee yleisia ammoniumnitraatin valmistukseen ja kemiaan liittyvia seikkoja sek\u00e4 erityisesti sen seitsem\u00e4\u00e4 kiderakennetta. Eri rakenteet ja niiden v\u00e4liset transitiot esitell\u00e4\u00e4n painopisteen ollessa rakenteille tunnusomaisessa dynaamisessa ep\u00e4jarjest\u00e4ytymisess\u00e4. Eri tutkijoiden antamien ristiriitaisten tietojen pohjalta on hahmotettu kosteuden merkityst\u00e4 transitioihin. T\u00e4rkeimm\u00e4t keskustelua synnytt\u00e4neet erimielisyydet liittyv\u00e4t kosteuden merkitykseen IV <=> III-transition esiintymiselle. Eri tutkijoiden raporteista syntyy k\u00e4sitys, ett\u00e4 kosteuden m\u00e4\u00e4r\u00e4 ei ole m\u00e4\u00e4r\u00e4\u00e4v\u00e4 tekij\u00e4, mutta kosteudella selv\u00e4stikin on merkityst\u00e4. Kirjallisuudesta ei selvi\u00e4 tarkemmin, mitk\u00e4 kosteuden aiheuttamat tekij\u00e4t vaikuttavat transition esiintymiseen tai sen tapahtumislamp\u00f6tilaan. \r\n\r\nKosteuden lis\u00e4ksi tiedet\u00e4\u00e4n n\u00e4ytteen termisen historian vaikuttavan IV <=> III-faasitransition esiintymiseen. Joidenkin tutkijoiden mielest\u00e4 termiset k\u00e4sittelyt vaikuttavat IV- ja II-faasin ep\u00e4j\u00e4rjest\u00e4ytymiseen. J\u00e4rjest\u00e4ytyneimm\u00e4t n\u00e4ytteet kulkisivat ohi III-faasin l\u00e4mmityksess\u00e4 ja j\u00e4\u00e4hdytyksess\u00e4, jolloin syntyy IV <=> II-transitio. Todisteita n\u00e4ille rakenteellisille seikoille on haettu huonohkolla menestyksell\u00e4 NMR-relaksaatioaikamittauksilla ja diffraktiomenetelmill\u00e4. V\u00e4rahtelyspektroskooppiset mittaukset antavat aihetta olettaa ep\u00e4j\u00e4rjest\u00e4ytymisen liittyv\u00e4n heteroionisen kytkeytymisen voimakkuuteen. \r\n\r\nRakenteiden ja transitioiden lis\u00e4ksi k\u00e4sitell\u00e4\u00e4n ammoniumnitraatin termodynaamisia ja kineettisi\u00e4 tutkimuksia. Erityisesti kineettiset tekij\u00e4t vaikuttavat t\u00e4rkeilt\u00e4 ajatellen ammoniumnitraatin kiinte\u00e4n olomuodon teknisi\u00e4 sovelluksia: sopivilla lis\u00e4aineilla III \r\n-> IV-transitiota hidastamalla lienee mahdollista valmistaa tuotteita, joissa toistuvissa l\u00e4mmitys-j\u00e4\u00e4hdytyssykleiss\u00e4 ei tapahdu lannoiterakeita rikkovia faasitransitioita. \r\n\r\nKokeellisessa osassa esitell\u00e4\u00e4n differentiaaliskannauskalorimetrin DSC ja r\u00f6ntgenpulveridiffraktiometrin RPD k\u00e4ytt\u00f6 ammoniumnitraatin faasitransitioiden tunnistamisessa ja transitiol\u00e4mp\u00f6tilojen, entalpiamuutosten ja l\u00e4mp\u00f6kapasiteetin muutosten mittaamisessa. Kehiteltyj\u00e4 menetelmi\u00e4 on k\u00e4ytetty havainnoitaessa faasitransitioreitin valintaa ja eri tekij\u00f6iden vaikutusta siihen. Transitioreittej\u00e4 IV-, III- ja II-faasin v\u00e4lill\u00e4 erilaisin variaatioin havaittiin kymmenen. Kosteuden m\u00e4\u00e4r\u00e4 ei vaikuttanut reitinvalintaan: n\u00e4ytteet saattoivat kulkea mit\u00e4 reitti\u00e4 tahansa riippumatta veden konsentraatiosta. Kosteuden v\u00e4heneminen II-faasin esiintymisl\u00e4mp\u00f6tilassa vaikutti IV -> II-transition muuttumiseen IV -> III-transitioksi. Kosteuden lis\u00e4\u00e4misell\u00e4 on saman suuntainen vaikutus. Muita transitioreitin valintaan vaikuttavia tekij\u00f6it\u00e4 olivat j\u00e4\u00e4hdytysnopeus n\u00e4ytteen valmistuksessa, n\u00e4ytteen ik\u00e4 ja yleens\u00e4 kaikki tekij\u00e4t, joiden yleens\u00e4 tiedet\u00e4\u00e4n vaikuttavan kiteisten aineiden j\u00e4rjestaytymisasteeseen. Hyvin j\u00e4rjest\u00e4ytyneet n\u00e4ytteet kulkisivat t\u00e4m\u00e4n mukaan IV <=> II-reitti\u00e4 ja huonommin j\u00e4rjestaytyneet IV <=> III <=> II-reitti\u00e4. J\u00e4rjest\u00e4ytymisastetta yritettiin m\u00e4\u00e4ritt\u00e4\u00e4 1\r\nRPD:lla, 1H-NMR:lla ja Raman-spektroskoopilla huonoin 17O- ja 15\r\nN-tuloksin. L\u00e4hitulevaisuudessa aloitetaan 170- ja 15N\u00adNMR-mittaukset ja jatketaan Raman-mittauksia erotuskyvylt\u00e4\u00e4n paremmilla laitteistoilla. Ammonimnitraatin kidefaasitransitioiden kineettisi\u00e4 tekij\u00f6it\u00e4 selvitettiin alustavasti. T\u00e4h\u00e4nkin aiheeseen palataan jatkotutkimuksissa l\u00e4hinn\u00e4 isotermisin\u00e4 DSC-mittauksina.", "language": "fi", "element": "description", "qualifier": "abstract", "schema": "dc"}, {"key": "dc.description.abstract", "value": "Crystal phase transitions of ammonium nitrate\r\n\r\n\r\nThe text is divided into literature review and experimental part. The literature review deals with general chemistry and especially with the seven crystal structures of ammonium nitrate. The structures and transitions between them are presented emphasis laying on the dynamical disorder of the structures. The effect of moisture is reviewed on the basis of contradictions in the literature, most important being the effect of water on the appearance of phase transition IV < = > III. It is easy to see that the content of water is not the ruling parameter, although water clearly has a role in the path selection. The role has not been clarified in the literature. \r\n\r\n\r\nExcept moisture the thermal history of a sample is known to effect on the appearance of phase transition IV < = > III. Some authors have the opinion that thermal treatments effect the degree of disorder of phases IV and II. The most ordered samples would pass phase III while heating or cooling, so that transitions IV < = > II would take place instead of IV < = > III. Evidences for these structural parameters are collected with NMR relaxation time measurements and with diffraction methods. Vibrational spectroscopy measurements give a reason to suppose that disorder is connected with the strength of heteroionic coupling. Except the structures and the transitions the text deals with thermodynamic and kinetic studies. Especially the kinetic factors seems to be important when one thinks about the technical applications of ammonium nitrate in solid state. With suitable additives it is most clearly possible to prepare products that doesn't go through the phase transitions that break the fertilizer granules.\r\n\r\nIn the experimental part of the work there are presented the use of differential scanning calorimetry DSC and X-ray powder diffraction XPD in identifying phase transitions of ammonium nitrate, and measuring transition temperatures, energies and changes of heat capacity of ammonium nitrate. The methods developed are used in studies on transition path selection and factors effecting on the selection. There was ten transition paths observed between phases IV, III and II in all. The amount of moisture did not effect on the path selection: samples could choose any of the ten paths regardless of the moisture concentration. Diminishing the moisture in the temperature of phase II changed the path IV - > II to path IV - > III. Increase of the water content had an effect of the same trend. Other observed factors effecting the path selection were the rate of cooling during the preparing of the samples, the age of the samples, and in general all the factors which are known to effect on the degree of order of crystals. Well ordered samples. would select path IV < = > II and less ordered path IV < = > III < = > II. Some not successful efforts were done on studying the degree of order with XPD, solid state 1H NMR and Raman spectroscopy. In the future there will be studies with 110 and 15N NMR and Raman spectroscopy with higher resolution. The kinetics of phase transitions of ammonium nitrate were examined in minor scale. The subject will be studied more closely with isothermal DSC.", "language": "en", "element": "description", "qualifier": "abstract", "schema": "dc"}, {"key": "dc.description.provenance", "value": "Submitted using Plone Publishing form by Miia Hakanen (mihakane) on 2017-06-20 09:59:31.279670. Form: Admin-lomake opinn\u00e4ytteiden julkaisuun (https://kirjasto.jyu.fi/julkaisut/julkaisulomakkeet/admin-lomake-opinnaytteet). 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