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Separation And Analysis Of Thermally Dissolved Products From Zhaotong Lignite And Wucaiwan Long Flame Coal Using Chromatographic Methods

Posted on:2018-07-28Degree:MasterType:Thesis
Country:ChinaCandidate:J L XiaFull Text:PDF
GTID:2321330539475320Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
Zhaotong lignite(ZL)and Wucaiwan long flame coal(WLFC)were sequentially dissoluted at 300 oC to afford soluble portions(SPs).SPs were separated and analyzed by three chromatographic methods,gas chromatography-mass spectrometry(GC-MS),comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry(GC×GC-TOF MS),and high-performance liquid chromatography time-of-flight mass spectrometry(HPLC-TOF MS).In the meantime,SPs were separated by silica gel column chromatography and the subfractions were analyzed using GC-MS.The GC-MS analytical results of SPs indicate that the ralative abundances of alkanes,arenes and phenols were higher in cyclohexane-thermal soluble portions.In acetone-thermal soluble portions,a higher ralative abundance of phorone was detected.For methonal-thermal soluble portions,higher ralative abundances of alcohols and phenols were detected.After further separation of each SPs by column chromatography,all kinds of fractions were enriched and mainly include: alkanes,aromatics in cyclohexane-thermal soluble portions and phorone in acetone-thermal soluble portions.GC×GC is one of the most powerful separational tools,because it has two capillary columus with different polarities to separate complex substances.When GC×GC is coupled with TOF MS,the deconvolution of some overlapping peaks and identification of compounds with close m/z become possible.Anlytical results of the acetone SPs of WLFC via GC×GC-TOF MS were discussed in-depth.GC×GC-TOF MS is more suitable for the characterization of polycyclic aromatic hydrocarbons,oxygen-containing,nitrogen-containing and sulfur compounds with relatively low abundance,due to its high peak capacity,high sensitivity and high resoloving power.Heteroatomic compounds in SPs were well detected by HPLC-ESI-TOF MS because of the ionization selectivity of ESI source.Some isomers in the SPs were separated and identified by HPLC-TOF MS,and the corresponding structural informations were proposed.Oxygen-containing compounds are thought to be mainly hydroxyl and carbonyl groups in SPs.Nitrogen-containing compounds in SPs were identified in the form of pyridine ring and amino.Sulfur-containing species mainly exist in sulfane and thiophene.
Keywords/Search Tags:coal, thermal dissolution, column chromatography, gas chromatography/mass spectrometry, comprehensive two-dimensional gas chromatography/time of flight mass spectrometry, high-performance liquid chromatography/ time-of-flight mass spectrometry
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