Preparation of low molecular weight cyclic polystyrenes with high purity via liquid chromatography at the critical condition
Cyclic polymers synthesized by ring-closure method from linear precursors contain some of linear contaminates. In this work, the origin of linear contaminates in cyclic polystyrenes (c-PS) is demonstrated by the coupling of liquid chromatography at the critical condition (LCCC) with matrix-assisted...
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| Veröffentlicht in: | Polymer (Guilford) 2018-01, Vol.135, p.279-284 |
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| creator | Gao, Lingfeng Oh, Joongsuk Tu, Yingfeng Chang, Taihyun |
| description | Cyclic polymers synthesized by ring-closure method from linear precursors contain some of linear contaminates. In this work, the origin of linear contaminates in cyclic polystyrenes (c-PS) is demonstrated by the coupling of liquid chromatography at the critical condition (LCCC) with matrix-assisted laser desorption/ionization time-of-flight mass spectra. The linear contaminates are revealed to be the “dead” chains during ATRP by chain termination, the unreacted linear polystyrene (l-PS) precursors, and the dimers by the imperfect ring-closure reaction. The c-PS are purified by LCCC fractionation, and the results show the LCCC fractionation at the critical adsorption point (CAP) of c-PS is more efficient than that at the CAP of linears for low molecular weight (99.6%) via the tandem-coupled LCCC fractionation at the CAP of l-PS and at the CAP of c-PS.
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•The linear contaminates in cyclic polystyrenes (c-PS) were identified.•The LCCC fractionation at the CAP of c-PS is very efficient.•Highly purified c-PS were obtained by a tandem-coupled LCCC fractionation method. |
| doi_str_mv | 10.1016/j.polymer.2017.12.020 |
| format | Article |
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[Display omitted]
•The linear contaminates in cyclic polystyrenes (c-PS) were identified.•The LCCC fractionation at the CAP of c-PS is very efficient.•Highly purified c-PS were obtained by a tandem-coupled LCCC fractionation method.</description><identifier>ISSN: 0032-3861</identifier><identifier>EISSN: 1873-2291</identifier><identifier>DOI: 10.1016/j.polymer.2017.12.020</identifier><language>eng</language><publisher>Kidlington: Elsevier Ltd</publisher><subject>Adsorption ; Chemical synthesis ; Chromatography ; Contamination ; Coupling (molecular) ; Cyclic polymer ; Dimers ; Fractionation ; Ionization ; Liquid chromatography ; Liquid chromatography at critical condition ; Low molecular weights ; Mass spectra ; Mathematical analysis ; Matrix methods ; Molecular weight ; Polymers ; Polystyrene ; Polystyrene resins ; Precursors ; Purity</subject><ispartof>Polymer (Guilford), 2018-01, Vol.135, p.279-284</ispartof><rights>2017 Elsevier Ltd</rights><rights>Copyright Elsevier BV Jan 17, 2018</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c337t-4137b70b618520391969a83580ef877bc8166cb78e1a03a39859800ee61377893</citedby><cites>FETCH-LOGICAL-c337t-4137b70b618520391969a83580ef877bc8166cb78e1a03a39859800ee61377893</cites><orcidid>0000-0001-6221-9145</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.polymer.2017.12.020$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3550,27924,27925,45995</link.rule.ids></links><search><creatorcontrib>Gao, Lingfeng</creatorcontrib><creatorcontrib>Oh, Joongsuk</creatorcontrib><creatorcontrib>Tu, Yingfeng</creatorcontrib><creatorcontrib>Chang, Taihyun</creatorcontrib><title>Preparation of low molecular weight cyclic polystyrenes with high purity via liquid chromatography at the critical condition</title><title>Polymer (Guilford)</title><description>Cyclic polymers synthesized by ring-closure method from linear precursors contain some of linear contaminates. In this work, the origin of linear contaminates in cyclic polystyrenes (c-PS) is demonstrated by the coupling of liquid chromatography at the critical condition (LCCC) with matrix-assisted laser desorption/ionization time-of-flight mass spectra. The linear contaminates are revealed to be the “dead” chains during ATRP by chain termination, the unreacted linear polystyrene (l-PS) precursors, and the dimers by the imperfect ring-closure reaction. The c-PS are purified by LCCC fractionation, and the results show the LCCC fractionation at the critical adsorption point (CAP) of c-PS is more efficient than that at the CAP of linears for low molecular weight (<10,000) PS. A two-step LCCC method is presented for the preparation of c-PS with high purity (>99.6%) via the tandem-coupled LCCC fractionation at the CAP of l-PS and at the CAP of c-PS.
[Display omitted]
•The linear contaminates in cyclic polystyrenes (c-PS) were identified.•The LCCC fractionation at the CAP of c-PS is very efficient.•Highly purified c-PS were obtained by a tandem-coupled LCCC fractionation method.</description><subject>Adsorption</subject><subject>Chemical synthesis</subject><subject>Chromatography</subject><subject>Contamination</subject><subject>Coupling (molecular)</subject><subject>Cyclic polymer</subject><subject>Dimers</subject><subject>Fractionation</subject><subject>Ionization</subject><subject>Liquid chromatography</subject><subject>Liquid chromatography at critical condition</subject><subject>Low molecular weights</subject><subject>Mass spectra</subject><subject>Mathematical analysis</subject><subject>Matrix methods</subject><subject>Molecular weight</subject><subject>Polymers</subject><subject>Polystyrene</subject><subject>Polystyrene resins</subject><subject>Precursors</subject><subject>Purity</subject><issn>0032-3861</issn><issn>1873-2291</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2018</creationdate><recordtype>article</recordtype><recordid>eNqFkE9LxDAUxIMouK5-BCHgufUl2TbpSUT8B4Ie9Byy2bc2S7epSepS8MObZb17eoeZ3wxvCLlkUDJg9fWmHHw3bTGUHJgsGS-BwxGZMSVFwXnDjskMQPBCqJqdkrMYNwDAK76YkZ-3gIMJJjnfU7-mnd_Rre_Qjp0JdIfus03UTrZzlu5bYpoC9hjpzqWWtlmmwxhcmui3M7RzX6NbUdsGvzXJfwYztBM1iaYWqc02Z01Hre9Xbl94Tk7Wpot48Xfn5OPh_v3uqXh5fXy-u30prBAyFQsm5FLCsmaq4iAa1tSNUaJSgGsl5dIqVtd2KRUyA8KIRlWNAkCsMyhVI-bk6pA7BP81Ykx648fQ50qdF1uIheSyyq7q4LLBxxhwrYfgtiZMmoHeD603-m_oPSY14zoPnbmbA4f5hW-X1Wgd9hZXLqBNeuXdPwm_QdCLIw</recordid><startdate>20180117</startdate><enddate>20180117</enddate><creator>Gao, Lingfeng</creator><creator>Oh, Joongsuk</creator><creator>Tu, Yingfeng</creator><creator>Chang, Taihyun</creator><general>Elsevier Ltd</general><general>Elsevier BV</general><scope>AAYXX</scope><scope>CITATION</scope><scope>7QF</scope><scope>7QO</scope><scope>7QQ</scope><scope>7SC</scope><scope>7SE</scope><scope>7SP</scope><scope>7SR</scope><scope>7T7</scope><scope>7TA</scope><scope>7TB</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>C1K</scope><scope>F28</scope><scope>FR3</scope><scope>H8D</scope><scope>H8G</scope><scope>JG9</scope><scope>JQ2</scope><scope>KR7</scope><scope>L7M</scope><scope>L~C</scope><scope>L~D</scope><scope>P64</scope><orcidid>https://orcid.org/0000-0001-6221-9145</orcidid></search><sort><creationdate>20180117</creationdate><title>Preparation of low molecular weight cyclic polystyrenes with high purity via liquid chromatography at the critical condition</title><author>Gao, Lingfeng ; Oh, Joongsuk ; Tu, Yingfeng ; Chang, Taihyun</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c337t-4137b70b618520391969a83580ef877bc8166cb78e1a03a39859800ee61377893</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2018</creationdate><topic>Adsorption</topic><topic>Chemical synthesis</topic><topic>Chromatography</topic><topic>Contamination</topic><topic>Coupling (molecular)</topic><topic>Cyclic polymer</topic><topic>Dimers</topic><topic>Fractionation</topic><topic>Ionization</topic><topic>Liquid chromatography</topic><topic>Liquid chromatography at critical condition</topic><topic>Low molecular weights</topic><topic>Mass spectra</topic><topic>Mathematical analysis</topic><topic>Matrix methods</topic><topic>Molecular weight</topic><topic>Polymers</topic><topic>Polystyrene</topic><topic>Polystyrene resins</topic><topic>Precursors</topic><topic>Purity</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Gao, Lingfeng</creatorcontrib><creatorcontrib>Oh, Joongsuk</creatorcontrib><creatorcontrib>Tu, Yingfeng</creatorcontrib><creatorcontrib>Chang, Taihyun</creatorcontrib><collection>CrossRef</collection><collection>Aluminium Industry Abstracts</collection><collection>Biotechnology Research Abstracts</collection><collection>Ceramic Abstracts</collection><collection>Computer and Information Systems Abstracts</collection><collection>Corrosion Abstracts</collection><collection>Electronics & Communications Abstracts</collection><collection>Engineered Materials Abstracts</collection><collection>Industrial and Applied Microbiology Abstracts (Microbiology A)</collection><collection>Materials Business File</collection><collection>Mechanical & Transportation Engineering Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Environmental Sciences and Pollution Management</collection><collection>ANTE: Abstracts in New Technology & Engineering</collection><collection>Engineering Research Database</collection><collection>Aerospace Database</collection><collection>Copper Technical Reference Library</collection><collection>Materials Research Database</collection><collection>ProQuest Computer Science Collection</collection><collection>Civil Engineering Abstracts</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>Computer and Information Systems Abstracts Academic</collection><collection>Computer and Information Systems Abstracts Professional</collection><collection>Biotechnology and BioEngineering Abstracts</collection><jtitle>Polymer (Guilford)</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Gao, Lingfeng</au><au>Oh, Joongsuk</au><au>Tu, Yingfeng</au><au>Chang, Taihyun</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Preparation of low molecular weight cyclic polystyrenes with high purity via liquid chromatography at the critical condition</atitle><jtitle>Polymer (Guilford)</jtitle><date>2018-01-17</date><risdate>2018</risdate><volume>135</volume><spage>279</spage><epage>284</epage><pages>279-284</pages><issn>0032-3861</issn><eissn>1873-2291</eissn><abstract>Cyclic polymers synthesized by ring-closure method from linear precursors contain some of linear contaminates. In this work, the origin of linear contaminates in cyclic polystyrenes (c-PS) is demonstrated by the coupling of liquid chromatography at the critical condition (LCCC) with matrix-assisted laser desorption/ionization time-of-flight mass spectra. The linear contaminates are revealed to be the “dead” chains during ATRP by chain termination, the unreacted linear polystyrene (l-PS) precursors, and the dimers by the imperfect ring-closure reaction. The c-PS are purified by LCCC fractionation, and the results show the LCCC fractionation at the critical adsorption point (CAP) of c-PS is more efficient than that at the CAP of linears for low molecular weight (<10,000) PS. A two-step LCCC method is presented for the preparation of c-PS with high purity (>99.6%) via the tandem-coupled LCCC fractionation at the CAP of l-PS and at the CAP of c-PS.
[Display omitted]
•The linear contaminates in cyclic polystyrenes (c-PS) were identified.•The LCCC fractionation at the CAP of c-PS is very efficient.•Highly purified c-PS were obtained by a tandem-coupled LCCC fractionation method.</abstract><cop>Kidlington</cop><pub>Elsevier Ltd</pub><doi>10.1016/j.polymer.2017.12.020</doi><tpages>6</tpages><orcidid>https://orcid.org/0000-0001-6221-9145</orcidid></addata></record> |
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| source | Elsevier ScienceDirect Journals |
| subjects | Adsorption Chemical synthesis Chromatography Contamination Coupling (molecular) Cyclic polymer Dimers Fractionation Ionization Liquid chromatography Liquid chromatography at critical condition Low molecular weights Mass spectra Mathematical analysis Matrix methods Molecular weight Polymers Polystyrene Polystyrene resins Precursors Purity |
| title | Preparation of low molecular weight cyclic polystyrenes with high purity via liquid chromatography at the critical condition |
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