Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2
Identifieur interne : 001125 ( Pmc/Curation ); précédent : 001124; suivant : 001126Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2
Auteurs : Jerzy J. Chru Ciel [Pologne] ; Marzena Fejdy ; Witold FortuniakSource :
- Polymers [ 2073-4360 ] ; 2018.
Abstract
Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO4/2 (Q), both MeHSiO (DH) and Me2SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me3SiO0.5 (M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150–155 °C. Yields of PMHS-Q reached from 55–69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7–13.1 cP. Molecular weights (MW) of PMHS-Q (Mn = 2440–6310 g/mol, Mw = 5750–10,350 g/mol) and polydispersities of MW (Mw/Mn = 2.0–2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, 1H- and 29Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of 29Si-NMR results and compared with literature data.
Url:
DOI: 10.3390/polym10050484
PubMed: 30966518
PubMed Central: 6415389
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO<sub>4/2</sub></title><author><name sortKey="Chru Ciel, Jerzy J" sort="Chru Ciel, Jerzy J" uniqKey="Chru Ciel J" first="Jerzy J." last="Chru Ciel">Jerzy J. Chru Ciel</name><affiliation wicri:level="1"><nlm:aff id="af1-polymers-10-00484">Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź, Poland</nlm:aff><country xml:lang="fr">Pologne</country><wicri:regionArea>Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź</wicri:regionArea></affiliation></author><author><name sortKey="Fejdy, Marzena" sort="Fejdy, Marzena" uniqKey="Fejdy M" first="Marzena" last="Fejdy">Marzena Fejdy</name><affiliation><nlm:aff id="af2-polymers-10-00484">The Institute of Security Technologies “MORATEX”, Marii Skłodowskiej-Curie Str. 3, 90-505 Łódź, Poland;<email>mfejdys@moratex.eu</email></nlm:aff></affiliation></author><author><name sortKey="Fortuniak, Witold" sort="Fortuniak, Witold" uniqKey="Fortuniak W" first="Witold" last="Fortuniak">Witold Fortuniak</name><affiliation><nlm:aff id="af3-polymers-10-00484">Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza Str. 112, 90-363 Łódź, Poland;<email>wfortuni@cbmm.lodz.pl</email></nlm:aff></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">30966518</idno><idno type="pmc">6415389</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC6415389</idno><idno type="RBID">PMC:6415389</idno><idno type="doi">10.3390/polym10050484</idno><date when="2018">2018</date><idno type="wicri:Area/Pmc/Corpus">001125</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">001125</idno><idno type="wicri:Area/Pmc/Curation">001125</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Curation">001125</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO<sub>4/2</sub></title><author><name sortKey="Chru Ciel, Jerzy J" sort="Chru Ciel, Jerzy J" uniqKey="Chru Ciel J" first="Jerzy J." last="Chru Ciel">Jerzy J. Chru Ciel</name><affiliation wicri:level="1"><nlm:aff id="af1-polymers-10-00484">Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź, Poland</nlm:aff><country xml:lang="fr">Pologne</country><wicri:regionArea>Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź</wicri:regionArea></affiliation></author><author><name sortKey="Fejdy, Marzena" sort="Fejdy, Marzena" uniqKey="Fejdy M" first="Marzena" last="Fejdy">Marzena Fejdy</name><affiliation><nlm:aff id="af2-polymers-10-00484">The Institute of Security Technologies “MORATEX”, Marii Skłodowskiej-Curie Str. 3, 90-505 Łódź, Poland;<email>mfejdys@moratex.eu</email></nlm:aff></affiliation></author><author><name sortKey="Fortuniak, Witold" sort="Fortuniak, Witold" uniqKey="Fortuniak W" first="Witold" last="Fortuniak">Witold Fortuniak</name><affiliation><nlm:aff id="af3-polymers-10-00484">Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza Str. 112, 90-363 Łódź, Poland;<email>wfortuni@cbmm.lodz.pl</email></nlm:aff></affiliation></author></analytic><series><title level="j">Polymers</title><idno type="eISSN">2073-4360</idno><imprint><date when="2018">2018</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO<sub>4/2</sub> (Q), both MeHSiO (D<sup>H</sup>) and Me<sub>2</sub>SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me<sub>3</sub>SiO<sub>0.5</sub> (M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150–155 °C. Yields of PMHS-Q reached from 55–69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7–13.1 cP. Molecular weights (MW) of PMHS-Q (M<sub>n</sub> = 2440–6310 g/mol, M<sub>w</sub> = 5750–10,350 g/mol) and polydispersities of MW (M<sub>w</sub>/M<sub>n</sub> = 2.0–2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, <sup>1</sup>H- and <sup>29</sup>Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of <sup>29</sup>Si-NMR results and compared with literature data.</p></div></front><back><div1 type="bibliography"><listBibl><biblStruct><analytic><author><name sortKey="Eaborn, C" uniqKey="Eaborn C">C. Eaborn</name></author></analytic></biblStruct><biblStruct><analytic><author><name sortKey="Noll, W" uniqKey="Noll W">W. 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<front><journal-meta><journal-id journal-id-type="nlm-ta">Polymers (Basel)</journal-id><journal-id journal-id-type="iso-abbrev">Polymers (Basel)</journal-id><journal-id journal-id-type="publisher-id">polymers</journal-id><journal-title-group><journal-title>Polymers</journal-title></journal-title-group><issn pub-type="epub">2073-4360</issn><publisher><publisher-name>MDPI</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="pmid">30966518</article-id><article-id pub-id-type="pmc">6415389</article-id><article-id pub-id-type="doi">10.3390/polym10050484</article-id><article-id pub-id-type="publisher-id">polymers-10-00484</article-id><article-categories><subj-group subj-group-type="heading"><subject>Article</subject></subj-group></article-categories><title-group><article-title>Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO<sub>4/2</sub></article-title></title-group><contrib-group><contrib contrib-type="author"><contrib-id contrib-id-type="orcid" authenticated="true">https://orcid.org/0000-0002-6227-9428</contrib-id><name><surname>Chruściel</surname><given-names>Jerzy J.</given-names></name><xref ref-type="aff" rid="af1-polymers-10-00484">1</xref><xref rid="c1-polymers-10-00484" ref-type="corresp">*</xref></contrib><contrib contrib-type="author"><name><surname>Fejdyś</surname><given-names>Marzena</given-names></name><xref ref-type="aff" rid="af2-polymers-10-00484">2</xref></contrib><contrib contrib-type="author"><contrib-id contrib-id-type="orcid" authenticated="true">https://orcid.org/0000-0002-4064-6944</contrib-id><name><surname>Fortuniak</surname><given-names>Witold</given-names></name><xref ref-type="aff" rid="af3-polymers-10-00484">3</xref></contrib></contrib-group><aff id="af1-polymers-10-00484"><label>1</label>Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź, Poland</aff><aff id="af2-polymers-10-00484"><label>2</label>The Institute of Security Technologies “MORATEX”, Marii Skłodowskiej-Curie Str. 3, 90-505 Łódź, Poland;<email>mfejdys@moratex.eu</email></aff><aff id="af3-polymers-10-00484"><label>3</label>Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza Str. 112, 90-363 Łódź, Poland;<email>wfortuni@cbmm.lodz.pl</email></aff><author-notes><corresp id="c1-polymers-10-00484"><label>*</label>Correspondence: <email>jchrusci@p.lodz.pl</email> or <email>jchrusciel@iw.lodz.pl</email>; Tel.: +48-42-61-63-187; Fax: +48-42-67-92-638</corresp></author-notes><pub-date pub-type="epub"><day>28</day><month>4</month><year>2018</year></pub-date><pub-date pub-type="collection"><month>5</month><year>2018</year></pub-date><volume>10</volume><issue>5</issue><elocation-id>484</elocation-id><history><date date-type="received"><day>28</day><month>3</month><year>2018</year></date><date date-type="accepted"><day>25</day><month>4</month><year>2018</year></date></history><permissions><copyright-statement>© 2018 by the authors.</copyright-statement><copyright-year>2018</copyright-year><license license-type="open-access"><license-p>Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (<ext-link ext-link-type="uri" xlink:href="http://creativecommons.org/licenses/by/4.0/">http://creativecommons.org/licenses/by/4.0/</ext-link>).</license-p></license></permissions><abstract><p>Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO<sub>4/2</sub> (Q), both MeHSiO (D<sup>H</sup>) and Me<sub>2</sub>SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me<sub>3</sub>SiO<sub>0.5</sub> (M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150–155 °C. Yields of PMHS-Q reached from 55–69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7–13.1 cP. Molecular weights (MW) of PMHS-Q (M<sub>n</sub> = 2440–6310 g/mol, M<sub>w</sub> = 5750–10,350 g/mol) and polydispersities of MW (M<sub>w</sub>/M<sub>n</sub> = 2.0–2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, <sup>1</sup>H- and <sup>29</sup>Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of <sup>29</sup>Si-NMR results and compared with literature data.</p></abstract><kwd-group><kwd>hyperbranched poly(methylhydrosiloxanes)</kwd><kwd>hydrolytic polycondensation</kwd><kwd><sup>29</sup>Si-NMR</kwd><kwd>topology of polysiloxane chains</kwd></kwd-group></article-meta></front><floats-group><fig id="polymers-10-00484-f001" orientation="portrait" position="float"><label>Figure 1</label><caption><p>FTIR spectrum of Q<sub>2</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub>.</p></caption><graphic xlink:href="polymers-10-00484-g001"></graphic></fig><fig id="polymers-10-00484-f002" orientation="portrait" position="float"><label>Figure 2</label><caption><p>FTIR spectrum of Q<sub>3</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub>.</p></caption><graphic xlink:href="polymers-10-00484-g002"></graphic></fig><fig id="polymers-10-00484-f003" orientation="portrait" position="float"><label>Figure 3</label><caption><p>FTIR spectrum of Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub>.</p></caption><graphic xlink:href="polymers-10-00484-g003"></graphic></fig><fig id="polymers-10-00484-f004" orientation="portrait" position="float"><label>Figure 4</label><caption><p><sup>1</sup>H-NMR spectrum (in C<sub>6</sub>D<sub>6</sub>) of polymethylhydrosiloxane Q<sub>3</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub>.</p></caption><graphic xlink:href="polymers-10-00484-g004"></graphic></fig><fig id="polymers-10-00484-f005" orientation="portrait" position="float"><label>Figure 5</label><caption><p><sup>29</sup>Si-NMR spectrum (INVGATE, in C<sub>6</sub>D<sub>6</sub>) of polymethylhydrosiloxane Q<sub>3</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub>.</p></caption><graphic xlink:href="polymers-10-00484-g005"></graphic></fig><fig id="polymers-10-00484-f006" orientation="portrait" position="float"><label>Figure 6</label><caption><p><sup>1</sup>H-NMR spectrum (in C<sub>6</sub>D<sub>6</sub>) of polymethylhydrosiloxane Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub>.</p></caption><graphic xlink:href="polymers-10-00484-g006"></graphic></fig><fig id="polymers-10-00484-f007" orientation="portrait" position="float"><label>Figure 7</label><caption><p><sup>29</sup>Si-NMR spectra (in C<sub>6</sub>D<sub>6</sub>) of polymethylhydrosiloxane Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub>: (<bold>a</bold>) INEPT, (<bold>b</bold>) INVGATE.</p></caption><graphic xlink:href="polymers-10-00484-g007"></graphic></fig><table-wrap id="polymers-10-00484-t001" orientation="portrait" position="float"><object-id pub-id-type="pii">polymers-10-00484-t001_Table 1</object-id><label>Table 1</label><caption><p>Amounts of substrates and a solvent, reaction time in syntheses of branched PMHS containing quadruple branching points, and methods of drying of products solutions.</p></caption><table frame="hsides" rules="groups"><thead><tr><th rowspan="3" colspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin">Substrates, solvent, and reaction conditions</th><th colspan="6" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">Predicted molecular formulas of PMHS-Q *</th></tr><tr><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">QD<sup>H</sup><sub>48</sub>M<sub>4</sub></th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Q<sub>2</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub></th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Q<sub>3</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub></th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">QD<sub>52</sub>D<sup>H</sup><sub>52</sub>M<sub>4</sub></th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub></th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Q<sub>3</sub>D<sub>50</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub></th></tr><tr><th colspan="6" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">Amounts of reagents and a solvent</th></tr></thead><tbody><tr><td rowspan="2" align="center" valign="middle" colspan="1"><bold>Si(OEt)<sub>4</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">(mol)</td><td align="center" valign="middle" rowspan="1" colspan="1">0.01</td><td align="center" valign="middle" rowspan="1" colspan="1">0.04</td><td align="center" valign="middle" rowspan="1" colspan="1">0.06</td><td align="center" valign="middle" rowspan="1" colspan="1">0.01</td><td align="center" valign="middle" rowspan="1" colspan="1">0.02</td><td align="center" valign="middle" rowspan="1" colspan="1">0.03</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">(cm<sup>3</sup>)</td><td align="center" valign="middle" rowspan="1" colspan="1">2.2</td><td align="center" valign="middle" rowspan="1" colspan="1">8.9</td><td align="center" valign="middle" rowspan="1" colspan="1">13.4</td><td align="center" valign="middle" rowspan="1" colspan="1">2.2</td><td align="center" valign="middle" rowspan="1" colspan="1">4.6</td><td align="center" valign="middle" rowspan="1" colspan="1">6.7</td></tr><tr><td rowspan="2" align="center" valign="middle" colspan="1"><bold>MeHSiCl<sub>2</sub> (MDS)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">(mol)</td><td align="center" valign="middle" rowspan="1" colspan="1">0.48</td><td align="center" valign="middle" rowspan="1" colspan="1">0.98</td><td align="center" valign="middle" rowspan="1" colspan="1">1.0</td><td align="center" valign="middle" rowspan="1" colspan="1">0.52</td><td align="center" valign="middle" rowspan="1" colspan="1">0.49</td><td align="center" valign="middle" rowspan="1" colspan="1">0.50</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">(cm<sup>3</sup>)</td><td align="center" valign="middle" rowspan="1" colspan="1">50.0</td><td align="center" valign="middle" rowspan="1" colspan="1">102.0</td><td align="center" valign="middle" rowspan="1" colspan="1">104.1</td><td align="center" valign="middle" rowspan="1" colspan="1">54.1</td><td align="center" valign="middle" rowspan="1" colspan="1">51.5</td><td align="center" valign="middle" rowspan="1" colspan="1">52.1</td></tr><tr><td rowspan="2" align="center" valign="middle" colspan="1"><bold>Me<sub>2</sub>SiCl<sub>2</sub> (DDS)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">(mol)</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">0.52</td><td align="center" valign="middle" rowspan="1" colspan="1">0.49</td><td align="center" valign="middle" rowspan="1" colspan="1">0.50</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">(cm<sup>3</sup>)</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">63.1</td><td align="center" valign="middle" rowspan="1" colspan="1">59.8</td><td align="center" valign="middle" rowspan="1" colspan="1">60.6</td></tr><tr><td rowspan="2" align="center" valign="middle" colspan="1"><bold>Me<sub>3</sub>SiCl (TMCS)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">(mol)</td><td align="center" valign="middle" rowspan="1" colspan="1">0.04</td><td align="center" valign="middle" rowspan="1" colspan="1">0.12</td><td align="center" valign="middle" rowspan="1" colspan="1">0.16</td><td align="center" valign="middle" rowspan="1" colspan="1">0.04</td><td align="center" valign="middle" rowspan="1" colspan="1">0.06</td><td align="center" valign="middle" rowspan="1" colspan="1">0.08</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">(cm<sup>3</sup>)</td><td align="center" valign="middle" rowspan="1" colspan="1">5.1</td><td align="center" valign="middle" rowspan="1" colspan="1">15.2</td><td align="center" valign="middle" rowspan="1" colspan="1">20.3</td><td align="center" valign="middle" rowspan="1" colspan="1">5.1</td><td align="center" valign="middle" rowspan="1" colspan="1">7.6</td><td align="center" valign="middle" rowspan="1" colspan="1">10.2</td></tr><tr><td rowspan="2" align="center" valign="middle" colspan="1"><bold>H<sub>2</sub>O</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">(mol)</td><td align="center" valign="middle" rowspan="1" colspan="1">9.11</td><td align="center" valign="middle" rowspan="1" colspan="1">18.94</td><td align="center" valign="middle" rowspan="1" colspan="1">19.66</td><td align="center" valign="middle" rowspan="1" colspan="1">19.33</td><td align="center" valign="middle" rowspan="1" colspan="1">18.38</td><td align="center" valign="middle" rowspan="1" colspan="1">18.94</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">(cm<sup>3</sup>)</td><td align="center" valign="middle" rowspan="1" colspan="1">164</td><td align="center" valign="middle" rowspan="1" colspan="1">341</td><td align="center" valign="middle" rowspan="1" colspan="1">354</td><td align="center" valign="middle" rowspan="1" colspan="1">348</td><td align="center" valign="middle" rowspan="1" colspan="1">331</td><td align="center" valign="middle" rowspan="1" colspan="1">341</td></tr><tr><td rowspan="2" align="center" valign="middle" colspan="1"><bold>(4-dimethylamino)-pyridine (DMAP)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">(mol)</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">0.003</td><td align="center" valign="middle" rowspan="1" colspan="1">0.0109</td><td align="center" valign="middle" rowspan="1" colspan="1">0.0108</td><td align="center" valign="middle" rowspan="1" colspan="1">0.01</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">(g)</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">0.3665</td><td align="center" valign="middle" rowspan="1" colspan="1">1.3316</td><td align="center" valign="middle" rowspan="1" colspan="1">1.3194</td><td align="center" valign="middle" rowspan="1" colspan="1">1.2217</td></tr><tr><td rowspan="2" align="center" valign="middle" colspan="1"><bold>Et<sub>3</sub>N</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">(mol)</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">0.03</td><td align="center" valign="middle" rowspan="1" colspan="1">0.109</td><td align="center" valign="middle" rowspan="1" colspan="1">0.108</td><td align="center" valign="middle" rowspan="1" colspan="1">0.10</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">(cm<sup>3</sup>)</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">4.2</td><td align="center" valign="middle" rowspan="1" colspan="1">101.2</td><td align="center" valign="middle" rowspan="1" colspan="1">15.1</td><td align="center" valign="middle" rowspan="1" colspan="1">13.9</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">Diethyl ether</td><td align="center" valign="middle" rowspan="1" colspan="1">(cm<sup>3</sup>)</td><td align="center" valign="middle" rowspan="1" colspan="1">50</td><td align="center" valign="middle" rowspan="1" colspan="1">80</td><td align="center" valign="middle" rowspan="1" colspan="1">60</td><td align="center" valign="middle" rowspan="1" colspan="1">100</td><td align="center" valign="middle" rowspan="1" colspan="1">80</td><td align="center" valign="middle" rowspan="1" colspan="1">90</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">Addition time of chlorosilanes and Si(OEt)<sub>4</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">(min)</td><td align="center" valign="middle" rowspan="1" colspan="1">50</td><td align="center" valign="middle" rowspan="1" colspan="1">60</td><td align="center" valign="middle" rowspan="1" colspan="1">95</td><td align="center" valign="middle" rowspan="1" colspan="1">80</td><td align="center" valign="middle" rowspan="1" colspan="1">55</td><td align="center" valign="middle" rowspan="1" colspan="1">95</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">Temperature during addition of chlorosilanes and Si(OEt)<sub>4</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">(°C)</td><td align="center" valign="middle" rowspan="1" colspan="1">−4–−2</td><td align="center" valign="middle" rowspan="1" colspan="1">−1–3</td><td align="center" valign="middle" rowspan="1" colspan="1">−1–3</td><td align="center" valign="middle" rowspan="1" colspan="1">−1–3</td><td align="center" valign="middle" rowspan="1" colspan="1">−1–6</td><td align="center" valign="middle" rowspan="1" colspan="1">−2–2</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">Stirring time after addition of chlorosilanes and Si(OEt)<sub>4</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">(min)</td><td align="center" valign="middle" rowspan="1" colspan="1">170</td><td align="center" valign="middle" rowspan="1" colspan="1">130</td><td align="center" valign="middle" rowspan="1" colspan="1">130</td><td align="center" valign="middle" rowspan="1" colspan="1">130</td><td align="center" valign="middle" rowspan="1" colspan="1">120</td><td align="center" valign="middle" rowspan="1" colspan="1">120</td></tr><tr><td colspan="2" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">Drying of products:</td><td colspan="3" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">with anhydrous MgSO<sub>4</sub></td><td colspan="3" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">by cooling in a fridge</td></tr></tbody></table><table-wrap-foot><fn><p>* Average molecular composition of polymers, based on a stoichiometry of monomers. PMHS-Q: liquid branched poly(methylhydrosiloxanes) of random structures.</p></fn></table-wrap-foot></table-wrap><table-wrap id="polymers-10-00484-t002" orientation="portrait" position="float"><object-id pub-id-type="pii">polymers-10-00484-t002_Table 2</object-id><label>Table 2</label><caption><p>Yields of PMHS-Q, conditions of removal of volatile products, and results of measurements of dynamic viscosity of branched PMHS, containing quadruple branching units Q.</p></caption><table frame="hsides" rules="groups"><thead><tr><th colspan="3" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">PMHS-Q</th><th rowspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" colspan="1">Dynamic viscosity</th><th colspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">Evacuation conditions</th><th colspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">Volatile products</th></tr><tr><th rowspan="2" align="center" valign="middle" style="border-bottom:solid thin" colspan="1">Predicted molecular formula (polymer abreviation)</th><th colspan="2" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">Yield</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Bath temp. </th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Time</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">B.p./pressure</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Mass</th></tr><tr><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">(g)</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">(wt%)</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">(cP)</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">(°C)</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">(min)</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">(°C/mm Hg)</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">(g)</th></tr></thead><tbody><tr><td align="left" valign="middle" rowspan="1" colspan="1"><bold>QD<sup>H</sup><sub>48</sub>M<sub>4</sub> (Q1)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">20.14</td><td align="center" valign="middle" rowspan="1" colspan="1">62</td><td align="center" valign="middle" rowspan="1" colspan="1">12.8</td><td align="center" valign="middle" rowspan="1" colspan="1">152</td><td align="center" valign="middle" rowspan="1" colspan="1">190</td><td align="center" valign="middle" rowspan="1" colspan="1">24/16–79/3.5</td><td align="center" valign="middle" rowspan="1" colspan="1">9.27</td></tr><tr><td align="left" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>2</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub> (Q2)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">48.70</td><td align="center" valign="middle" rowspan="1" colspan="1">68</td><td align="center" valign="middle" rowspan="1" colspan="1">11.0</td><td align="center" valign="middle" rowspan="1" colspan="1">154</td><td align="center" valign="middle" rowspan="1" colspan="1">200</td><td align="center" valign="middle" rowspan="1" colspan="1">23/16–77/3.5</td><td align="center" valign="middle" rowspan="1" colspan="1">18.14</td></tr><tr><td align="left" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>3</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub> (Q3)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">52.82</td><td align="center" valign="middle" rowspan="1" colspan="1">69</td><td align="center" valign="middle" rowspan="1" colspan="1">13.1</td><td align="center" valign="middle" rowspan="1" colspan="1">155</td><td align="center" valign="middle" rowspan="1" colspan="1">190</td><td align="center" valign="middle" rowspan="1" colspan="1">23/18–70/3.5</td><td align="center" valign="middle" rowspan="1" colspan="1">16.71</td></tr><tr><td align="left" valign="middle" rowspan="1" colspan="1"><bold>QD<sub>52</sub>D<sup>H</sup><sub>52</sub>M<sub>4</sub> (Q1D)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">40.29</td><td align="center" valign="middle" rowspan="1" colspan="1">55</td><td align="center" valign="middle" rowspan="1" colspan="1">12.5</td><td align="center" valign="middle" rowspan="1" colspan="1">150</td><td align="center" valign="middle" rowspan="1" colspan="1">210</td><td align="center" valign="middle" rowspan="1" colspan="1">21/21–80/5</td><td align="center" valign="middle" rowspan="1" colspan="1">34.84</td></tr><tr><td align="left" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub> (Q2D)</bold></td><td align="center" valign="middle" rowspan="1" colspan="1">40.49</td><td align="center" valign="middle" rowspan="1" colspan="1">56</td><td align="center" valign="middle" rowspan="1" colspan="1">11.8</td><td align="center" valign="middle" rowspan="1" colspan="1">155</td><td align="center" valign="middle" rowspan="1" colspan="1">200</td><td align="center" valign="middle" rowspan="1" colspan="1">27/19–78/4</td><td align="center" valign="middle" rowspan="1" colspan="1">31.06</td></tr><tr><td align="left" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1"><bold>Q<sub>3</sub>D<sub>50</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub> (Q3D)</bold></td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">43.77</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">58</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">10.7</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">155</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">190</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">21/16–74/4.5</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">28.22</td></tr></tbody></table></table-wrap><table-wrap id="polymers-10-00484-t003" orientation="portrait" position="float"><object-id pub-id-type="pii">polymers-10-00484-t003_Table 3</object-id><label>Table 3</label><caption><p>Characteristics of polymethylhydrosiloxanes with branched, random structure of siloxane chains, containing branching units Q.</p></caption><table frame="hsides" rules="groups"><thead><tr><th rowspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" colspan="1">PMHS-Q</th><th rowspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" colspan="1">M<sub>n</sub> (calc.)</th><th rowspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" colspan="1">M<sub>n</sub></th><th rowspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" colspan="1">M<sub>w</sub></th><th rowspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" colspan="1">M<sub>w</sub>/M<sub>n</sub></th><th colspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">% C</th><th colspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">% H</th><th colspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">% Si</th></tr><tr><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">calc.</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">found</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">calc.</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">found</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">calc.</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">found</th></tr></thead><tbody><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>QD<sup>H</sup><sub>48</sub>M<sub>4</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">3271</td><td align="center" valign="middle" rowspan="1" colspan="1">6310</td><td align="center" valign="middle" rowspan="1" colspan="1">17,750</td><td align="center" valign="middle" rowspan="1" colspan="1">2.81</td><td align="center" valign="middle" rowspan="1" colspan="1">22.03</td><td align="center" valign="middle" rowspan="1" colspan="1">21.51<break></break>21.76</td><td align="center" valign="middle" rowspan="1" colspan="1">7.03</td><td align="center" valign="middle" rowspan="1" colspan="1">6.61<break></break>6.90</td><td align="center" valign="middle" rowspan="1" colspan="1">45.50</td><td align="center" valign="middle" rowspan="1" colspan="1">44.87</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>2</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">3554</td><td align="center" valign="middle" rowspan="1" colspan="1">3220</td><td align="center" valign="middle" rowspan="1" colspan="1">8330</td><td align="center" valign="middle" rowspan="1" colspan="1">2.59</td><td align="center" valign="middle" rowspan="1" colspan="1">22.64</td><td align="center" valign="middle" rowspan="1" colspan="1">22.01<break></break>22.11</td><td align="center" valign="middle" rowspan="1" colspan="1">7.09</td><td align="center" valign="middle" rowspan="1" colspan="1">6.92<break></break>7.01</td><td align="center" valign="middle" rowspan="1" colspan="1">45.05</td><td align="center" valign="middle" rowspan="1" colspan="1">45.15</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>3</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">3836</td><td align="center" valign="middle" rowspan="1" colspan="1">3840</td><td align="center" valign="middle" rowspan="1" colspan="1">10,350</td><td align="center" valign="middle" rowspan="1" colspan="1">2.69</td><td align="center" valign="middle" rowspan="1" colspan="1">23.16</td><td align="center" valign="middle" rowspan="1" colspan="1">22.03<break></break>22.14</td><td align="center" valign="middle" rowspan="1" colspan="1">7.14</td><td align="center" valign="middle" rowspan="1" colspan="1">7.02<break></break>6.85</td><td align="center" valign="middle" rowspan="1" colspan="1">44.65</td><td align="center" valign="middle" rowspan="1" colspan="1">43.81</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>QD<sub>52</sub>D<sup>H</sup><sub>52</sub>M<sub>4</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">7367</td><td align="center" valign="middle" rowspan="1" colspan="1">2650</td><td align="center" valign="middle" rowspan="1" colspan="1">6280</td><td align="center" valign="middle" rowspan="1" colspan="1">2.36</td><td align="center" valign="middle" rowspan="1" colspan="1">27.39</td><td align="center" valign="middle" rowspan="1" colspan="1">28.89<break></break>28.70</td><td align="center" valign="middle" rowspan="1" colspan="1">7.60</td><td align="center" valign="middle" rowspan="1" colspan="1">7.89<break></break>8.03</td><td align="center" valign="middle" rowspan="1" colspan="1">41.55</td><td align="center" valign="middle" rowspan="1" colspan="1">41.54</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">7187</td><td align="center" valign="middle" rowspan="1" colspan="1">2440</td><td align="center" valign="middle" rowspan="1" colspan="1">5750</td><td align="center" valign="middle" rowspan="1" colspan="1">2.35</td><td align="center" valign="middle" rowspan="1" colspan="1">27.57</td><td align="center" valign="middle" rowspan="1" colspan="1">28.15<break></break>28.40</td><td align="center" valign="middle" rowspan="1" colspan="1">7.63</td><td align="center" valign="middle" rowspan="1" colspan="1">7.69<break></break>7.88</td><td align="center" valign="middle" rowspan="1" colspan="1">41.42</td><td align="center" valign="middle" rowspan="1" colspan="1">41.40</td></tr><tr><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1"><bold>Q<sub>3</sub>D<sub>50</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub></bold></td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">7544</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">5100</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">10,210</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">2.00</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">27.07</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">27.78<break></break>27.92</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">7.65</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">8.35<break></break>7.98</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">41.32</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">41.30</td></tr></tbody></table></table-wrap><table-wrap id="polymers-10-00484-t004" orientation="portrait" position="float"><object-id pub-id-type="pii">polymers-10-00484-t004_Table 4</object-id><label>Table 4</label><caption><p>Characteristic absorption bands in FTIR spectra of Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub>.</p></caption><table frame="hsides" rules="groups"><thead><tr><th colspan="2" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">Wave number [cm<sup>−1</sup>]</th><th align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1" colspan="1">Group or bond</th><th align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1" colspan="1">Vibration</th></tr></thead><tbody><tr><td align="center" valign="middle" rowspan="1" colspan="1">found</td><td align="center" valign="middle" rowspan="1" colspan="1">literature data [<xref rid="B72-polymers-10-00484" ref-type="bibr">72</xref>] </td><td align="center" valign="middle" rowspan="1" colspan="1"></td><td align="center" valign="middle" rowspan="1" colspan="1"></td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">2965</td><td align="center" valign="middle" rowspan="1" colspan="1">2975–2950</td><td align="center" valign="middle" rowspan="1" colspan="1">CH<sub>3</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">ν <sub>asym</sub> C-H</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">2878</td><td align="center" valign="middle" rowspan="1" colspan="1">2885–2860</td><td align="center" valign="middle" rowspan="1" colspan="1">CH<sub>3</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">ν <sub>sym</sub> C-H</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">2164</td><td align="center" valign="middle" rowspan="1" colspan="1">2300–2100</td><td align="center" valign="middle" rowspan="1" colspan="1">Si-H</td><td align="center" valign="middle" rowspan="1" colspan="1">ν Si-H</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">1450</td><td align="center" valign="middle" rowspan="1" colspan="1">1470–1420</td><td align="center" valign="middle" rowspan="1" colspan="1">CH<sub>3</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">δ <sub>asym</sub> C-H</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">1410</td><td align="center" valign="middle" rowspan="1" colspan="1">1390–1365</td><td align="center" valign="middle" rowspan="1" colspan="1">CH<sub>3</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">δ <sub>sym</sub> C-H</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">1260</td><td align="center" valign="middle" rowspan="1" colspan="1">1265–1250</td><td align="center" valign="middle" rowspan="1" colspan="1">Si-CH<sub>3</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">δ <sub>asym</sub> Si-C</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">1115–1027</td><td align="center" valign="middle" rowspan="1" colspan="1">1100–1000</td><td align="center" valign="middle" rowspan="1" colspan="1">Si-O-Si</td><td align="center" valign="middle" rowspan="1" colspan="1">ν <sub>asym</sub> Si-O</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">910</td><td align="center" valign="middle" rowspan="1" colspan="1">950–800</td><td align="center" valign="middle" rowspan="1" colspan="1">Si-H</td><td align="center" valign="middle" rowspan="1" colspan="1">δ Si-H</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">864</td><td align="center" valign="middle" rowspan="1" colspan="1">860–750</td><td align="center" valign="middle" rowspan="1" colspan="1">Si-CH<sub>3</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">ν <sub>asym</sub> Si-C</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">830</td><td align="center" valign="middle" rowspan="1" colspan="1">910–830</td><td align="center" valign="middle" rowspan="1" colspan="1">Si-O</td><td align="center" valign="middle" rowspan="1" colspan="1">ν <sub>asym</sub> Si-O</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1">800</td><td align="center" valign="middle" rowspan="1" colspan="1">800</td><td align="center" valign="middle" rowspan="1" colspan="1">Si-CH<sub>3</sub></td><td align="center" valign="middle" rowspan="1" colspan="1">δ <sub>sym</sub> Si-C</td></tr><tr><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">759</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">755</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Si-(CH<sub>3</sub>)<sub>3</sub></td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">δ <sub>asym</sub> Si-C</td></tr></tbody></table></table-wrap><table-wrap id="polymers-10-00484-t005" orientation="portrait" position="float"><object-id pub-id-type="pii">polymers-10-00484-t005_Table 5</object-id><label>Table 5</label><caption><p>Chemical shifts of PMHS-Q in their <sup>1</sup>H- and <sup>29</sup>Si-NMR spectra (in C6D6).</p></caption><table frame="hsides" rules="groups"><thead><tr><th rowspan="4" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" colspan="1">PMHS-Q</th><th colspan="11" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">δ (ppm)</th></tr><tr><th rowspan="2" colspan="2" align="center" valign="middle" style="border-bottom:solid thin"><sup>1</sup>H-NMR</th><th colspan="9" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1"><sup>29</sup>Si-NMR</th></tr><tr><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">INEPT</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">INVGATE</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">INEPT</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">INVGATE</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">INEPT</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">INVGATE</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">INEPT</th><th colspan="2" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">INVGATE</th></tr><tr><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Si–H</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">Si–CH<sub>3</sub></th><th colspan="2" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">Me<sub>3</sub>SiO<sub>0.5</sub></th><th colspan="2" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">Me<sub>2</sub>SiO</th><th colspan="2" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">MeHSiO</th><th colspan="2" align="center" valign="middle" style="border-bottom:solid thin" rowspan="1">MeSiO<sub>3/2</sub></th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">SiO<sub>4/2</sub></th></tr></thead><tbody><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>QD<sup>H</sup><sub>48</sub>M<sub>4</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">4.90</td><td align="center" valign="middle" rowspan="1" colspan="1">0.01–0.22</td><td align="center" valign="middle" rowspan="1" colspan="1">9.75–11.03</td><td align="center" valign="middle" rowspan="1" colspan="1">9.98–10.96</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">−31.51–−37.42</td><td align="center" valign="middle" rowspan="1" colspan="1">−31.85–−35.90</td><td align="center" valign="middle" rowspan="1" colspan="1">−64.51</td><td align="center" valign="middle" rowspan="1" colspan="1">−64.58</td><td align="center" valign="middle" rowspan="1" colspan="1">−101.40–−108.13</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>2</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">4.80</td><td align="center" valign="middle" rowspan="1" colspan="1">0.01–0.12</td><td align="center" valign="middle" rowspan="1" colspan="1">9.40–11.24</td><td align="center" valign="middle" rowspan="1" colspan="1">9.70–10.32</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">−31.62–−39.97</td><td align="center" valign="middle" rowspan="1" colspan="1">−31.83–−36.25</td><td align="center" valign="middle" rowspan="1" colspan="1">−62.60–−64.61</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">−101.37–−112.33</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>3</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">4.80</td><td align="center" valign="middle" rowspan="1" colspan="1">0.01–0.12</td><td align="center" valign="middle" rowspan="1" colspan="1">9.40–11.25</td><td align="center" valign="middle" rowspan="1" colspan="1">9.42–11.28</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">-</td><td align="center" valign="middle" rowspan="1" colspan="1">−37.46–−31.16</td><td align="center" valign="middle" rowspan="1" colspan="1">−32.16–−35.87</td><td align="center" valign="middle" rowspan="1" colspan="1">−62.97–−64.56</td><td align="center" valign="middle" rowspan="1" colspan="1">−64.54</td><td align="center" valign="middle" rowspan="1" colspan="1">−100.31–−110.20</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>QD<sub>52</sub>D<sup>H</sup><sub>52</sub>M<sub>4</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">4.92</td><td align="center" valign="middle" rowspan="1" colspan="1">0.05–0.22</td><td align="center" valign="middle" rowspan="1" colspan="1">9.92–7.27</td><td align="center" valign="middle" rowspan="1" colspan="1">7.30–9.96</td><td align="center" valign="middle" rowspan="1" colspan="1">−18.48–−21.74</td><td align="center" valign="middle" rowspan="1" colspan="1">−18.67–−21.44</td><td align="center" valign="middle" rowspan="1" colspan="1">−33.27–−38.87</td><td align="center" valign="middle" rowspan="1" colspan="1">−34.56–−37.30</td><td align="center" valign="middle" rowspan="1" colspan="1">−63.12–−65.39</td><td align="center" valign="middle" rowspan="1" colspan="1">−63.72–−65.89</td><td align="center" valign="middle" rowspan="1" colspan="1">−102.92–−109.92</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><bold>Q<sub>2</sub>D<sub>49</sub>D<sup>H</sup><sub>49</sub>M<sub>6</sub></bold></td><td align="center" valign="middle" rowspan="1" colspan="1">4.92</td><td align="center" valign="middle" rowspan="1" colspan="1">0.01–0.30</td><td align="center" valign="middle" rowspan="1" colspan="1">9.92–7.26</td><td align="center" valign="middle" rowspan="1" colspan="1">7.32–9.98</td><td align="center" valign="middle" rowspan="1" colspan="1">−18.43–−21.85</td><td align="center" valign="middle" rowspan="1" colspan="1">−18.70–−21.69</td><td align="center" valign="middle" rowspan="1" colspan="1">−34.54–−37.33</td><td align="center" valign="middle" rowspan="1" colspan="1">−34.61–−37.03</td><td align="center" valign="middle" rowspan="1" colspan="1">−62.95–−65.26</td><td align="center" valign="middle" rowspan="1" colspan="1">−62.35–−66.16</td><td align="center" valign="middle" rowspan="1" colspan="1">−101.81–−109.71</td></tr><tr><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1"><bold>Q<sub>3</sub>D<sub>50</sub>D<sup>H</sup><sub>50</sub>M<sub>8</sub></bold></td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">4.83</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">0.01–0.23</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">9.91–7.27</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">7.32–9.98</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−18.77–−21.75</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−18.72–−21.29</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−34.61–−37.57</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−34.54–−36.10</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−64.73</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−63.35–−65.16</td><td align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−102.84–−109.61</td></tr></tbody></table></table-wrap><table-wrap id="polymers-10-00484-t006" orientation="portrait" position="float"><object-id pub-id-type="pii">polymers-10-00484-t006_Table 6</object-id><label>Table 6</label><caption><p>The microstructure of siloxane chains in PMHS-Q, containing quadruple branching units Q (all possible sequences among tetrads of terminal groups, and linear and star pentads); values of δ concern Si atoms in structural units denoted as bold and underlined.</p></caption><table frame="hsides" rules="groups"><thead><tr><th colspan="6" align="center" valign="middle" style="border-top:solid thin;border-bottom:solid thin" rowspan="1">δ <sup>29</sup>Si-NMR (ppm)</th></tr><tr><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">9–11</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">7–8</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−18–−19</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−20–−22</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−33–−37</th><th align="center" valign="middle" style="border-bottom:solid thin" rowspan="1" colspan="1">−101–−109</th></tr></thead><tbody><tr><td align="center" valign="top" style="border-bottom:solid thin" rowspan="1" colspan="1"><bold><underline>M</underline></bold>D<sup>H</sup>D<sup>H</sup>D<sup>H</sup><break></break><break></break><bold><underline>M</underline></bold>D<sup>H</sup>D<sup>H</sup>Q<break></break><break></break><bold><underline>M</underline></bold>D<sup>H</sup>QD<sup>H</sup><break></break><break></break><bold><underline>M</underline></bold>D<sup>H</sup>D<sup>H</sup>D<break></break><break></break><bold><underline>M</underline></bold>D<sup>H</sup>D<sup>H</sup>D<sup>H</sup><break></break><break></break><bold><underline>M</underline></bold>D<sup>H</sup>DD<sup>H</sup><break></break><break></break><bold><underline>M</underline></bold>D<sup>H</sup>DD</td><td align="center" valign="top" style="border-bottom:solid thin" rowspan="1" colspan="1"><bold><underline>M</underline></bold>DDD<break></break><break></break><bold><underline>M</underline></bold>DDD<sup>H</sup><break></break><break></break><bold><underline>M</underline></bold>DD<sup>H</sup>D<break></break><break></break><bold><underline>M</underline></bold>DD<sup>H</sup>D<sup>H</sup><break></break><break></break><bold><underline>M</underline></bold>DDQ<break></break><break></break><bold><underline>M</underline></bold>DQD<break></break><break></break><bold><underline>M</underline></bold>QDD<break></break><bold><underline>M</underline></bold>QDD<sup>H</sup></td><td align="center" valign="top" style="border-bottom:solid thin" rowspan="1" colspan="1">DD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>D<break></break><break></break>DD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>D<sup>H</sup><break></break><break></break>D<sup>H</sup>D<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>D<sup>H</sup><break></break><break></break>DD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>Q<break></break><break></break>QD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>Q<break></break><break></break>MD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>D<break></break><break></break>MD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>D<sup>H</sup><break></break><break></break>MD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>Q<break></break><break></break>MD<sup>H</sup><bold><underline>D</underline></bold>D<sup>H</sup>D</td><td align="center" valign="top" style="border-bottom:solid thin" rowspan="1" colspan="1">D<sup>H</sup>D<bold><underline>D</underline></bold>D<sup>H</sup>D<sup>H</sup><break></break>D<sup>H</sup>D<bold><underline>D</underline></bold>D<sup>H</sup>D<break></break>DD<bold><underline>D</underline></bold>D<sup>H</sup>D<sup>H</sup><break></break>DD<bold><underline>D</underline></bold>D<sup>H</sup>D<break></break>D<sup>H</sup>D<bold><underline>D</underline></bold>DQ<break></break>D<sup>H</sup>D<bold><underline>D</underline></bold>QD<break></break>DD<sup>H</sup><bold><underline>D</underline></bold>DQ<break></break>DD<sup>H</sup><bold><underline>D</underline></bold>QD<break></break>DD<bold><underline>D</underline></bold>DQ<break></break>DD<bold><underline>D</underline></bold>QD<break></break>QD<bold><underline>D</underline></bold>DQ<break></break>QD<bold><underline>D</underline></bold>QD<break></break>DQ<bold><underline>D</underline></bold>QD<break></break>DQ<bold><underline>D</underline></bold>DQ<break></break>MD<bold><underline>D</underline></bold>DQ<break></break>MD<bold><underline>D</underline></bold>QD<break></break>MQ<bold><underline>D</underline></bold>DD<break></break>MD<bold><underline>D</underline></bold>DQ<break></break>MQ<bold><underline>D</underline></bold>QD</td><td align="center" valign="top" style="border-bottom:solid thin" rowspan="1" colspan="1">D<sup>H</sup>D<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>D<sup>H</sup><break></break>DD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>D<sup>H</sup><break></break>D<sup>H</sup>D<bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>D<sup>H</sup><break></break>DD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>D <break></break>DD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>DD<sup>H</sup><break></break>D<sup>H</sup>D<bold><underline>D<sup>H</sup></underline></bold>D D<sup>H</sup><break></break>D<sup>H</sup>D<bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>Q <break></break>D<sup>H</sup>D<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>QD<sup>H</sup><break></break>DD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>Q<break></break>D<sup>H</sup>D<bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>Q <break></break>D<sup>H</sup>D<bold><underline>D<sup>H</sup></underline></bold>QD<sup>H</sup><break></break>DD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold><sup>H</sup>QD<sup>H</sup><break></break>DD<bold><underline>D<sup>H</sup></underline></bold>QD<sup>H</sup><break></break>D<sup>H</sup>D<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>DQ <break></break>D<sup>H</sup>D<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>QD<break></break>DD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>DQ<break></break>DD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>QD<break></break>D<sup>H</sup>D<bold><underline>D<sup>H</sup></underline></bold>DQ<break></break>D<sup>H</sup>D<bold><underline>D<sup>H</sup></underline></bold>QD<break></break>DD<bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>Q<break></break>DD<bold><underline>D<sup>H</sup></underline></bold>DQ<break></break>MD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>D<sup>H</sup><break></break>MD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup> D<break></break>MD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>DD<sup>H</sup><break></break>MD<bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>D<sup>H</sup><break></break>MD<bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>D<break></break>MD<bold><underline>D<sup>H</sup></underline></bold>DD<sup>H</sup><break></break>MD<sup>H</sup><bold><underline>D</underline></bold><sup>H</sup>D<sup>H</sup>Q<break></break>MD<bold><underline>D<sup>H</sup></underline></bold>D<sup>H</sup>Q<break></break>MD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>DQ<break></break>MD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>QD<break></break>MD<sup>H</sup><bold><underline>D<sup>H</sup></underline></bold>QD<sup>H</sup><break></break>MD<bold><underline>D<sup>H</sup></underline></bold>QD<sup>H</sup><break></break>MD<bold><underline>D<sup>H</sup></underline></bold>DQ</td><td align="center" valign="top" style="border-bottom:solid thin" rowspan="1" colspan="1"><break></break>D<break></break>D<bold><underline>Q</underline></bold>D<break></break>D<break></break><break></break><break></break>D<break></break>D<bold><underline>Q</underline></bold>D<break></break>M<break></break><break></break><break></break>D<break></break>D<bold><underline>Q</underline></bold>M<break></break>M<break></break><break></break><break></break>D<break></break>D<bold><underline>Q</underline></bold>D<sup>H</sup><break></break>D<break></break><break></break><break></break>D<break></break>D<bold><underline>Q</underline></bold>D<sup>H</sup><break></break>D<sup>H</sup><break></break><break></break><break></break>M<break></break>D<bold><underline>Q</underline></bold>D<break></break>D<sup>H</sup></td></tr></tbody></table></table-wrap></floats-group></pmc></record>Pour manipuler ce document sous Unix (Dilib)
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