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Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production / Geraint L. Sullivan

Swansea University Author: Geraint L. Sullivan

DOI (Published version): 10.23889/Suthesis.50204

Abstract

The identification and quantitation of organic tars, often requires specialised sampling techniques, such as gas sampling tubes, headspace vials and thermal desorption kits, which all require additional modules for instrument interfacing and sample introduction. The gold standard analysis techniques...

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Published: Swansea 2018
Institution: Swansea University
Degree level: Doctoral
Degree name: Ph.D
URI: https://cronfa.swan.ac.uk/Record/cronfa50204
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Sullivan</name><active>true</active><ethesisStudent>true</ethesisStudent></author></swanseaauthors><date>2019-05-02</date><abstract>The identification and quantitation of organic tars, often requires specialised sampling techniques, such as gas sampling tubes, headspace vials and thermal desorption kits, which all require additional modules for instrument interfacing and sample introduction. The gold standard analysis techniques for these organic gaseous compounds is gas chromatography coupled to mass spectrometry (GC-MS) as it provides separation of complex samples and high mass selectivity of ions. A solvent trap method using acetone to capture organic tars that originate from thermochemical treatment of different feedstocks; pinewood, brownfield soil (contaminated with oily sludge) and secondary treated sludge cake. It was then possible to analyse tar compounds without the expense of additional instrumentation and user training. Compounds identified in the solvent traps varied according to the feedstock used. Pine wood was used as an operational standard and generated typical biomass tars from sugar and lignin breakdown. Brownfield soil contaminated with oily sludge generated a wide range of polyaromatic hydrocarbons (PAHs), typical with hydrocarbon waste and secondary sludge cake generated a mixture of biomass breakdown products and nitrogenous compounds. Acetone provided a dual role, not only as a sample preparation method but for syngas cleaning. Tandem acetone scrubbers removed the majority of tars (&gt;90% efficiency) and also capable of removing troublesome volatile compounds, such as acetylene. Spent acetone scrubbers could easily be recycled using waste heat, with up to &gt;90% of semi-volatile tars being recovered. Clean syngas was converted to hydrocarbons using the Fischer-Tropsch (FT) reaction where a novel low temperature Cobalt was used. This catalyst was prepared in a different method from conventional cobalt catalysts (energy intensive calcination 12h at 600 ⁰C in air). The novel catalyst (CAT-1) was prepared using chemical oxidation to generate a cheaper and environmentally friendlier FT catalyst. Initial test experiments, using simulated syngas (bottled carbon monoxide and hydrogen) showed the generation of hydrocarbon material, suggesting a successful catalytic reaction. Further to this a trial using real scrubbed syngas from a combined gasification/ FT system, generated trace hydrocarbons, with no contamination in the final product from the tars, suggesting progress with acetone scrubbers. To further the economic feasibility of pyrolysis/gasification-FT process a smaller investigation into possible use of the remaining biochar as a sorbent to treat contaminated water simulating aqueous scrubbers. Biochar derived from pine wood and uncharacterised sludge cake were activated and showed selectivity for volatile polyaromatic compounds and petroleum derived compounds.</abstract><type>E-Thesis</type><journal/><volume/><journalNumber/><paginationStart/><paginationEnd/><publisher/><placeOfPublication>Swansea</placeOfPublication><isbnPrint/><isbnElectronic/><issnPrint/><issnElectronic/><keywords>Pyrolysis, gasification, Fisher-Tropsch, Gas chromatography-Mass spectrometery</keywords><publishedDay>31</publishedDay><publishedMonth>12</publishedMonth><publishedYear>2018</publishedYear><publishedDate>2018-12-31</publishedDate><doi>10.23889/Suthesis.50204</doi><url/><notes>Under embargo until 29/04/2024.</notes><college>COLLEGE NANME</college><department>Swansea University Medical School</department><CollegeCode>COLLEGE CODE</CollegeCode><institution>Swansea University</institution><degreelevel>Doctoral</degreelevel><degreename>Ph.D</degreename><degreesponsorsfunders>Decus Research</degreesponsorsfunders><apcterm/><funders/><projectreference/><lastEdited>2024-07-11T15:32:07.3396622</lastEdited><Created>2019-05-02T12:13:42.9366039</Created><path><level id="1">Faculty of Medicine, Health and Life Sciences</level><level id="2">Swansea University Medical School - Medicine</level></path><authors><author><firstname>Geraint L.</firstname><surname>Sullivan</surname><orcid>0000-0002-3370-2768</orcid><order>1</order></author></authors><documents><document><filename>0050204-02052019122940.pdf</filename><originalFilename>Sullivan_Geraint_L_PhD_Final_Thesis_Redacted_Signiture_Only.pdf</originalFilename><uploaded>2019-05-02T12:29:40.1830000</uploaded><type>Output</type><contentLength>3863111</contentLength><contentType>application/pdf</contentType><version>Redacted version - open access</version><cronfaStatus>true</cronfaStatus><embargoDate>2024-04-29T00:00:00.0000000</embargoDate><copyrightCorrect>true</copyrightCorrect><language>eng</language></document></documents><OutputDurs/></rfc1807>
spelling v2 50204 2019-05-02 Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production c3b9c5e1e6357330527c1a63a479b0f3 0000-0002-3370-2768 Geraint L. Sullivan Geraint L. Sullivan true true 2019-05-02 The identification and quantitation of organic tars, often requires specialised sampling techniques, such as gas sampling tubes, headspace vials and thermal desorption kits, which all require additional modules for instrument interfacing and sample introduction. The gold standard analysis techniques for these organic gaseous compounds is gas chromatography coupled to mass spectrometry (GC-MS) as it provides separation of complex samples and high mass selectivity of ions. A solvent trap method using acetone to capture organic tars that originate from thermochemical treatment of different feedstocks; pinewood, brownfield soil (contaminated with oily sludge) and secondary treated sludge cake. It was then possible to analyse tar compounds without the expense of additional instrumentation and user training. Compounds identified in the solvent traps varied according to the feedstock used. Pine wood was used as an operational standard and generated typical biomass tars from sugar and lignin breakdown. Brownfield soil contaminated with oily sludge generated a wide range of polyaromatic hydrocarbons (PAHs), typical with hydrocarbon waste and secondary sludge cake generated a mixture of biomass breakdown products and nitrogenous compounds. Acetone provided a dual role, not only as a sample preparation method but for syngas cleaning. Tandem acetone scrubbers removed the majority of tars (>90% efficiency) and also capable of removing troublesome volatile compounds, such as acetylene. Spent acetone scrubbers could easily be recycled using waste heat, with up to >90% of semi-volatile tars being recovered. Clean syngas was converted to hydrocarbons using the Fischer-Tropsch (FT) reaction where a novel low temperature Cobalt was used. This catalyst was prepared in a different method from conventional cobalt catalysts (energy intensive calcination 12h at 600 ⁰C in air). The novel catalyst (CAT-1) was prepared using chemical oxidation to generate a cheaper and environmentally friendlier FT catalyst. Initial test experiments, using simulated syngas (bottled carbon monoxide and hydrogen) showed the generation of hydrocarbon material, suggesting a successful catalytic reaction. Further to this a trial using real scrubbed syngas from a combined gasification/ FT system, generated trace hydrocarbons, with no contamination in the final product from the tars, suggesting progress with acetone scrubbers. To further the economic feasibility of pyrolysis/gasification-FT process a smaller investigation into possible use of the remaining biochar as a sorbent to treat contaminated water simulating aqueous scrubbers. Biochar derived from pine wood and uncharacterised sludge cake were activated and showed selectivity for volatile polyaromatic compounds and petroleum derived compounds. E-Thesis Swansea Pyrolysis, gasification, Fisher-Tropsch, Gas chromatography-Mass spectrometery 31 12 2018 2018-12-31 10.23889/Suthesis.50204 Under embargo until 29/04/2024. COLLEGE NANME Swansea University Medical School COLLEGE CODE Swansea University Doctoral Ph.D Decus Research 2024-07-11T15:32:07.3396622 2019-05-02T12:13:42.9366039 Faculty of Medicine, Health and Life Sciences Swansea University Medical School - Medicine Geraint L. Sullivan 0000-0002-3370-2768 1 0050204-02052019122940.pdf Sullivan_Geraint_L_PhD_Final_Thesis_Redacted_Signiture_Only.pdf 2019-05-02T12:29:40.1830000 Output 3863111 application/pdf Redacted version - open access true 2024-04-29T00:00:00.0000000 true eng
title Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production
spellingShingle Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production
Geraint L. Sullivan
title_short Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production
title_full Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production
title_fullStr Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production
title_full_unstemmed Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production
title_sort Application of gas chromatography-mass spectrometry (GC-MS) in the quantitative analysis of organic analytes generated in gasification/pyrolysis coupled Fischer Tropsch (FT) reactor: syngas clean-up and hydrocarbon production
author_id_str_mv c3b9c5e1e6357330527c1a63a479b0f3
author_id_fullname_str_mv c3b9c5e1e6357330527c1a63a479b0f3_***_Geraint L. Sullivan
author Geraint L. Sullivan
author2 Geraint L. Sullivan
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publishDate 2018
institution Swansea University
doi_str_mv 10.23889/Suthesis.50204
college_str Faculty of Medicine, Health and Life Sciences
hierarchytype
hierarchy_top_id facultyofmedicinehealthandlifesciences
hierarchy_top_title Faculty of Medicine, Health and Life Sciences
hierarchy_parent_id facultyofmedicinehealthandlifesciences
hierarchy_parent_title Faculty of Medicine, Health and Life Sciences
department_str Swansea University Medical School - Medicine{{{_:::_}}}Faculty of Medicine, Health and Life Sciences{{{_:::_}}}Swansea University Medical School - Medicine
document_store_str 1
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description The identification and quantitation of organic tars, often requires specialised sampling techniques, such as gas sampling tubes, headspace vials and thermal desorption kits, which all require additional modules for instrument interfacing and sample introduction. The gold standard analysis techniques for these organic gaseous compounds is gas chromatography coupled to mass spectrometry (GC-MS) as it provides separation of complex samples and high mass selectivity of ions. A solvent trap method using acetone to capture organic tars that originate from thermochemical treatment of different feedstocks; pinewood, brownfield soil (contaminated with oily sludge) and secondary treated sludge cake. It was then possible to analyse tar compounds without the expense of additional instrumentation and user training. Compounds identified in the solvent traps varied according to the feedstock used. Pine wood was used as an operational standard and generated typical biomass tars from sugar and lignin breakdown. Brownfield soil contaminated with oily sludge generated a wide range of polyaromatic hydrocarbons (PAHs), typical with hydrocarbon waste and secondary sludge cake generated a mixture of biomass breakdown products and nitrogenous compounds. Acetone provided a dual role, not only as a sample preparation method but for syngas cleaning. Tandem acetone scrubbers removed the majority of tars (>90% efficiency) and also capable of removing troublesome volatile compounds, such as acetylene. Spent acetone scrubbers could easily be recycled using waste heat, with up to >90% of semi-volatile tars being recovered. Clean syngas was converted to hydrocarbons using the Fischer-Tropsch (FT) reaction where a novel low temperature Cobalt was used. This catalyst was prepared in a different method from conventional cobalt catalysts (energy intensive calcination 12h at 600 ⁰C in air). The novel catalyst (CAT-1) was prepared using chemical oxidation to generate a cheaper and environmentally friendlier FT catalyst. Initial test experiments, using simulated syngas (bottled carbon monoxide and hydrogen) showed the generation of hydrocarbon material, suggesting a successful catalytic reaction. Further to this a trial using real scrubbed syngas from a combined gasification/ FT system, generated trace hydrocarbons, with no contamination in the final product from the tars, suggesting progress with acetone scrubbers. To further the economic feasibility of pyrolysis/gasification-FT process a smaller investigation into possible use of the remaining biochar as a sorbent to treat contaminated water simulating aqueous scrubbers. Biochar derived from pine wood and uncharacterised sludge cake were activated and showed selectivity for volatile polyaromatic compounds and petroleum derived compounds.
published_date 2018-12-31T15:32:07Z
_version_ 1804293454720663552
score 11.036553

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