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dc.contributor.authorMilne, John Noelen
dc.date.accessioned2019-02-15T14:37:12Z
dc.date.available2019-02-15T14:37:12Z
dc.date.issued1949
dc.identifier.urihttp://hdl.handle.net/1842/35347
dc.description.abstracten
dc.description.abstract#1. Efficient columns have been constructed for the fractional distillation of bases at atmospheric pressure and under precisely controlled vacuum. These include the following - a. 14 -Plate vacuum column (Eyelet Packing) - b. 40 -Plate column (Penske Helices) c. 100 -Plate vacuum column (I.C.I.gauze rings) d. 14- mm. column (I.C.I. gauze rings) Column a. was subsequently converted to 30- Plates by re- packing with I.C.I. gauze rings. Plate efficiency tests were carried out on columns a. and 'o. and estimates made of the efficiency of column c. A simple type of rotary fractional extraction apparatus has also been constructed. #2. A typical sample of "Basic Tar" from Pumpherston Oil Refinery was examined and found to contain so 40 per cent of volatile bases boiling up to 310°C at atmospheric pressure. 210 litres of "Basic Tar" were distilled under vacuum in a 16 -litre pot -still and 25 per cent (53 litres) of bases boiling up to 190°C at 20 mm. Hg. recovered. The bases were found to consist substantial of tertiary heterocyclic nitrogen compounds, the lower boiling ranges were mainly simple homologues of pyridine with methyl side chains. Quinolines are believed to be present in the higher ranges and more complex compounds are also thought to be present. #3. The bases were subjected to a series of systematic fractional distillations and ultimately bases boiling up to 210°C at atmospheric pressure were fractionated in a column of 100-theoretical plates. #4. Three ranges have been examined by chemical methods. These are Range 1, 169.9-171°C /760 mm.Hg Range 2, 186.1-188°C/760mm.Hg. and Range 3, 134.5-134.6°C/100mm.Hg. The following compounds were identified, 3:5-lutidine; 2:3:5-collidine; 2:4:5 -collidine; 2:4:6- collidine and 2:3:4:6- parvoline. Several compounds were isolated as crystalline derivatives, the identities of which have not been established. Two oily picrates were obtained, the bases regenerated from one of which had an unusually high refractive index and gave no crystalline derivatives. #5. Infra red absorption spectrograms have been obtained from several of the compounds isolated and these favour the proposed structures. #6. The dissociation constants of a series of pyridine and quinoline bases have been determined and discussed. #7. A survey has been made of the literature dealing with separation methods and this has been included as an appendix.en
dc.publisherThe University of Edinburghen
dc.relation.ispartofAnnexe Thesis Digitisation Project 2019 Block 22en
dc.relation.isreferencedbyen
dc.titleStudies in nitrogenous bases from Scottish shale oilen
dc.typeThesis or Dissertationen
dc.type.qualificationlevelDoctoralen
dc.type.qualificationnamePhD Doctor of Philosophyen


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