Name: reliable mechanochemistry: protocols for reproducible outcomes of neat and liquid assisted ball-mill grinding experiments
Uploaded: 2018-01-23T14:30:00
Description: Watch this Scientific Journal Video about Reliable Mechanochemistry: Protocols for Reproducible Outcomes of Neat and Liquid Assisted Ball-mill Grinding Experiments at JoVE.com

AMB и JKMS благодарна EPSRC для финансовой поддержки. Мы благодарим C. A. Bland за дизайн и механические установки и P. Доннелли для разработки программного обеспечения автоматизации Кофемолки для повторять шлифования. Мы благодарим Ричарда Соловей, Ollie Норрис и Симон Dowe механический цех для изготовления размольных, и электромагнитный держатель для установки «Нажмите кнопку» и Keith Парментер от мастерской стекла в Отдел химии для Производство стеклянных скольжениях образца PXRD. Мы благодарим C. A. Bland за техническое обслуживание и ремонт винт закрытия размольных стаканов. Мы благодарим профессор Билл Джонс для использования оборудования PXRD на кафедры химии и профессор Крис Хантер для использования его помещений лаборатории. Мы благодарим Отдел наук о земле (GIL) для общей поддержки.

1. Проверка точного дозирования органических растворителей
<ol><li>
Проверка точное дозирование органических растворителей в режиме обратного пипетки Примечание: Пипетки перемещения воздуха в реверсном режиме дозирования были отобраны для диапазона ЛАГ растворителей (ацето...

<ol>
	<li>James, S. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanochemistry:+opportunities+for+new+and+cleaner+synthesis.">Mechanochemistry: opportunities for new and cleaner synthesis.</a> Chem Soc Rev. 41 (1), 413-447 (2012).</li><li>Braga, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvent+effect+in+a+"solvent+free"+reaction.">Solvent effect in a "solvent free" reaction.</a> CrystEngComm. 9 (10), 879-881 (2007).</li><li>Karki, S., Friscic, T., Jones, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Control+and+interconversion+of+cocrystal+stoichiometry+in+grinding:+stepwise+mechanism+for+the+formation+of+a+hydrogen-bonded+cocrystal.">Control and interconversion of cocrystal stoichiometry in grinding: stepwise mechanism for the formation of a hydrogen-bonded cocrystal.</a> CrystEngComm. 11 (3), 470-481 (2009).</li><li>Kaupp, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solid-state+molecular+syntheses:+complete+reactions+without+auxiliaries+based+on+the+new+solid-state+mechanism.">Solid-state molecular syntheses: complete reactions without auxiliaries based on the new solid-state mechanism.</a> CrystEngComm. 5 (23), 117-133 (2003).</li><li>Biswal, B. P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanochemical+synthesis+of+chemically+stable+isoreticular+covalent+organic+frameworks.">Mechanochemical synthesis of chemically stable isoreticular covalent organic frameworks.</a> J Am Chem Soc. 135 (14), 5328-5331 (2013).</li><li>Garay, A. L., Pichon, A., James, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvent-free+synthesis+of+metal+complexes.">Solvent-free synthesis of metal complexes.</a> Chem Soc Rev. 36 (6), 846-855 (2007).</li><li>Kaupp, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanochemistry:+the+varied+applications+of+mechanical+bond-breaking.">Mechanochemistry: the varied applications of mechanical bond-breaking.</a> Cryst Eng Comm. 11 (3), 388-403 (2009).</li><li>Morris, R. E., James, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solventless+synthesis+of+zeolites.">Solventless synthesis of zeolites.</a> Angew Chem Int Ed Engl. 52 (8), 2163-2165 (2013).</li><li>Stolle, A., Szuppa, T., Leonhardt, S. E., Ondruschka, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ball+milling+in+organic+synthesis:+solutions+and+challenges.">Ball milling in organic synthesis: solutions and challenges.</a> Chem Soc Rev. 40 (5), 2317-2329 (2011).</li><li>Suryanarayana, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanical+alloying+and+milling.">Mechanical alloying and milling.</a> Prog Mater Sci. 46 (1-2), 1-184 (2001).</li><li>Wang, G. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanochemical+organic+synthesis.">Mechanochemical organic synthesis.</a> Chem Soc Rev. 42 (18), 7668-7700 (2013).</li><li>Braga, D., Grepioni, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reactions+between+or+within+molecular+crystals.">Reactions between or within molecular crystals.</a> Angew Chem Int Ed Engl. 43 (31), 4002-4011 (2004).</li><li>Friscic, T., Childs, S. L., Rizvi, S. A. A., Jones, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+role+of+solvent+in+mechanochemical+and+sonochemical+cocrystal+formation:+a+solubility-based+approach+for+predicting+cocrystallisation+outcome.">The role of solvent in mechanochemical and sonochemical cocrystal formation: a solubility-based approach for predicting cocrystallisation outcome.</a> Cryst Eng Comm. 11 (3), 418-426 (2009).</li><li>Fucke, K., Myz, S. A., Shakhtshneider, T. P., Boldyreva, E. V., Griesser, U. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=How+good+are+the+crystallisation+methods+for+co-crystals?+A+comparative+study+of+piroxicam.">How good are the crystallisation methods for co-crystals? A comparative study of piroxicam.</a> New J Chem. 36 (10), 1969-1977 (2012).</li><li>Bennett, T. D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Facile+mechanosynthesis+of+amorphous+zeolitic+imidazolate+frameworks.">Facile mechanosynthesis of amorphous zeolitic imidazolate frameworks.</a> J Am Chem Soc. 133 (37), 14546-14549 (2011).</li><li>Braga, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanochemical+preparation+of+molecular+and+supramolecular+organometallic+materials+and+coordination+networks.">Mechanochemical preparation of molecular and supramolecular organometallic materials and coordination networks.</a> Dalton Trans. (10), 1249-1263 (2006).</li><li>Yuan, W., Fri&#353;&#269;i&#263;, T., Apperley, D., James, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High+Reactivity+of+Metal-Organic+Frameworks+under+Grinding+Conditions:+Parallels+with+Organic+Molecular+Materials.">High Reactivity of Metal-Organic Frameworks under Grinding Conditions: Parallels with Organic Molecular Materials.</a> Angew Chem Int Ed Engl. 122 (23), 4008-4011 (2010).</li><li>Icli, B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+Molecular+Nanostructures+by+Multicomponent+Condensation+Reactions+in+a+Ball+Mill.">Synthesis of Molecular Nanostructures by Multicomponent Condensation Reactions in a Ball Mill.</a> J Am Chem Soc. 131 (9), 3154-3155 (2009).</li><li>Hsu, C. -. C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvent-free+synthesis+of+the+smallest+rotaxane+prepared+to+date.">Solvent-free synthesis of the smallest rotaxane prepared to date.</a> Angew Chem Int Ed Engl. 47 (39), 7475-7478 (2008).</li><li>Boldyreva, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanochemistry+of+inorganic+and+organic+systems:+what+is+similar,+what+is+different?.">Mechanochemistry of inorganic and organic systems: what is similar, what is different?.</a> Chem Soc Rev. 42 (18), 7719-7738 (2013).</li><li>Gracin, D., &#352;trukil, V., Fri&#353;&#269;i&#263;, T., Halasz, I., U&#382;arevi&#263;, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Laboratory+Real-Time+and+In+Situ+Monitoring+of+Mechanochemical+Milling+Reactions+by+Raman+Spectroscopy.">Laboratory Real-Time and In Situ Monitoring of Mechanochemical Milling Reactions by Raman Spectroscopy.</a> Angew Chem Int Ed Engl. 53 (24), 6193-6197 (2014).</li><li>Halasz, I., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+and+real-time+monitoring+of+mechanochemical+milling+reactions+using+synchrotron+X-ray+diffraction.">In situ and real-time monitoring of mechanochemical milling reactions using synchrotron X-ray diffraction.</a> Nat. Protocols. 8 (9), 1718-1729 (2013).</li><li>Ma, X., Yuan, W., Bell, S. E. J., James, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Better+understanding+of+mechanochemical+reactions:+Raman+monitoring+reveals+surprisingly+simple+'pseudo-fluid'+model+for+a+ball+milling+reaction.">Better understanding of mechanochemical reactions: Raman monitoring reveals surprisingly simple 'pseudo-fluid' model for a ball milling reaction.</a> Chem Commun. 50 (13), 1585-1587 (2014).</li><li>Tumanov, I. A., Michalchuk, A. A. L., Politov, A., Boldyreva, E., Boldyrev, V. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Inadvertent+Liquid+Assisted+Grinding:+A+Key+to+"Dry"+Organic+Mechano-Co-Crystallisation?.">Inadvertent Liquid Assisted Grinding: A Key to "Dry" Organic Mechano-Co-Crystallisation?.</a> CrystEngComm. 19, 2830-2835 (2017).</li><li>Belenguer, A. M., Lampronti, G. I., Cruz-Cabeza, A. J., Hunter, C. A., Sanders, J. K. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvation+and+surface+effects+on+polymorph+stabilities+at+the+nanoscale.">Solvation and surface effects on polymorph stabilities at the nanoscale.</a> Chem Sci. 7 (11), 6617-6627 (2016).</li><li>Belenguer, A. M., Friscic, T., Day, G. M., Sanders, J. K. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solid-state+dynamic+combinatorial+chemistry:+reversibility+and+thermodynamic+product+selection+in+covalent+mechanosynthesis.">Solid-state dynamic combinatorial chemistry: reversibility and thermodynamic product selection in covalent mechanosynthesis.</a> Chem Sci. 2 (4), 696-700 (2011).</li><li>Belenguer, A. M., Lampronti, G. I., Wales, D. J., Sanders, J. K. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Observation+of+Intermediates+in+a+Thermodynamically+Controlled+Solid-State+Dynamic+Covalent+Reaction.">Direct Observation of Intermediates in a Thermodynamically Controlled Solid-State Dynamic Covalent Reaction.</a> J Am Chem Soc. 136 (46), 16156-16166 (2014).</li><li>Evora, A. O. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resolved+structures+of+two+picolinamide+polymorphs.+Investigation+of+the+dimorphic+system+behaviour+under+conditions+relevant+to+co-crystal+synthesis.">Resolved structures of two picolinamide polymorphs. Investigation of the dimorphic system behaviour under conditions relevant to co-crystal synthesis.</a> CrystEngComm. 14 (24), 8649-8657 (2012).</li><li>Trask, A. V., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Selective+polymorph+transformation+via+solvent-drop+grinding.">Selective polymorph transformation via solvent-drop grinding.</a> Chemical Communications. (7), 880 (2005).</li><li>Hasa, D., Miniussi, E., Jones, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanochemical+Synthesis+of+Multicomponent+Crystals:+One+Liquid+for+One+Polymorph?+A+Myth+to+Dispel.">Mechanochemical Synthesis of Multicomponent Crystals: One Liquid for One Polymorph? A Myth to Dispel.</a> Cryst Growth Des. 16 (8), 4582-4588 (2016).</li><li>Hunter, C. A., Anderson, H. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=What+is+cooperativity?.">What is cooperativity?.</a> Angew Chem Int Ed Engl. 48 (41), 7488-7499 (2009).</li><li>McCusker, L. B., Dreele, R. B. V., Cox, D. E., Lou&#235;r, D., Scardi, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rietveld+refinement+guidelines.">Rietveld refinement guidelines.</a> J Appl Crystallogr. 32 (1), 36-50 (1999).</li><li>Allen, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Cambridge+Structural+Database:+a+quarter+of+a+million+crystal+structures+and+rising.">The Cambridge Structural Database: a quarter of a million crystal structures and rising.</a> Acta Crystallogr Sect B. 58 (3 Part 1), 380-388 (2002).</li><li>Gra&#382;ulis, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Crystallography+Open+Database-an+open-access+collection+of+crystal+structures.">Crystallography Open Database-an open-access collection of crystal structures.</a> J Appl Crystallogr. 42 (4), 726-729 (2009).</li><li>Cheary, R. W., Coelho, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+fundamental+parameters+approach+to+X-ray+line-profile+fitting.">A fundamental parameters approach to X-ray line-profile fitting.</a> J Appl Crystallogr. 25 (2), 109-121 (1992).</li><li>Tumanov, I. A., Michalchuk, A. A. L., Politov, A., Boldyreva, E., Boldyrev, V. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Inadvertent+Liquid+Assisted+Grinding:+A+Key+to+"Dry"+Organic+Mechano-Co-Crystallisation?.">Inadvertent Liquid Assisted Grinding: A Key to "Dry" Organic Mechano-Co-Crystallisation?.</a> CrystEngComm. 19, 2830-2835 (2017).</li><li>Batzdorf, L., Fischer, F., Wilke, M., Wenzel, K. J., Emmerling, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+In+Situ+Investigation+of+Milling+Reactions+Using+Combined+X-ray+Diffraction+and+Raman+Spectroscopy.">Direct In Situ Investigation of Milling Reactions Using Combined X-ray Diffraction and Raman Spectroscopy.</a> Angew Chem Int Ed Engl. 54 (6), 1799-1802 (2015).</li><li>Tumanov, N., Ban, V., Poulain, A., Filinchuk, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=3D-printed+jars+for+ball-milling+experiments+monitored+in+situ+by+X-ray+powder+diffraction.">3D-printed jars for ball-milling experiments monitored in situ by X-ray powder diffraction.</a> J Appl Crystallogr. 50 (4), 994-999 (2017).</li></ol>

Хотя большинство литературы по механохимии фокусируется на прагматических результатов или на механизмы реакции в настоящем документе рассматриваются конечную точку термодинамических мяч мельница помола. С этой точки зрения кинетические исследования являются необходимым шагом к оп...

<table>
	<tbody>
		<tr>
			<td>Bis(2-nitrophenyl) disulfide named 1-1</td>
			<td>Aldrich</td>
			<td>215228-25G</td>
			<td>[1155-00-6] 
			(98%)</td>
		</tr>
		<tr>
			<td>Bis(4-chlorophenyl) disulfide named 2-2</td>
			<td>TCI</td>
			<td>D0360</td>
			<td>[1142-19-4] 
			(98+%)</td>
		</tr>
		<tr>
			<td>1,8-Diazabicyclo [5.4.0]undec-7-ene (dbu)</td>
			<td>Acros Organics</td>
			<td>160610250</td>
			<td>[6674-22-2] 
			(&#62;97.5 % by GC)</td>
		</tr>
		<tr>
			<td>2-nitrophenyl-4-chlorophenyl-disulfide named 1-2</td>
			<td>in house synthesis</td>
			<td></td>
			<td>Synthesised by ball mill grinding: 1:1 of 1-1 + 2-2 + 2%M dbu</td>
		</tr>
		<tr>
			<td>Form A</td>
			<td>in house synthesis</td>
			<td></td>
			<td>Polymorph of 1-2 prepared by ball mill neat grinding</td>
		</tr>
		<tr>
			<td>Form B</td>
			<td>in house synthesis</td>
			<td></td>
			<td>Polymorph of 1-2 prepared by ball mill liquid assisted grinding</td>
		</tr>
		<tr>
			<td>Formic Acid</td>
			<td>Scientific Laboratory Supplies</td>
			<td>56302-50ML</td>
			<td>[64-18-6] 
			Mass spectrometry grade</td>
		</tr>
		<tr>
			<td>Trifluoroacetic acid (TFA)</td>
			<td>ThermoFisher</td>
			<td>85183</td>
			<td>[76-05-1] 
			Reagent-Plus 99%</td>
		</tr>
		<tr>
			<td>Water (H2O)</td>
			<td>Rathburn</td>
			<td>W/0106/PB17</td>
			<td>[7732-18-5] 
			HPLC gradient analysis grade used also for HPLC analysis</td>
		</tr>
		<tr>
			<td>Acetonitrile (MeCN),</td>
			<td>Merck</td>
			<td>160610250</td>
			<td>[75-05-8] 
			Hypergrade for LCMS grade LiChrosolv used also for HPLC analysis</td>
		</tr>
		<tr>
			<td>Acetone</td>
			<td>Fisher Scientific</td>
			<td>A/0606/17</td>
			<td>[67-64-1] 
			HPLC grade</td>
		</tr>
		<tr>
			<td>Methanol (MeOH)</td>
			<td>Fisher Scientific</td>
			<td>M/4062/17</td>
			<td>[67-56-1] 
			LCMS grade</td>
		</tr>
		<tr>
			<td>Ethanol (EtOH)</td>
			<td>Sigma Aldrich</td>
			<td>15727-5L</td>
			<td>[64-17-5] 
			laboratory reagent, absolute,</td>
		</tr>
		<tr>
			<td>isopropanol (IPA)</td>
			<td>Fisher Scientific</td>
			<td>P/7508/17</td>
			<td>[67-63-0] 
			HPLC grade</td>
		</tr>
		<tr>
			<td>Tetrahydrofurane (THF)</td>
			<td>Acros Organics</td>
			<td>268290010</td>
			<td>[109-99-9] 
			For HPLC; 99%8, unstabilised</td>
		</tr>
		<tr>
			<td>Ethyl acetate (EtOAc)</td>
			<td>Fisher Scientific</td>
			<td>E/0906/15</td>
			<td>[141-78-6]</td>
		</tr>
		<tr>
			<td>Chloroform (CHCl3,)</td>
			<td>Fisher Scientific</td>
			<td>C/4966/17</td>
			<td>[67-66-3] 
			HPLC grade, stabilised with amylene</td>
		</tr>
		<tr>
			<td>Dichloromethane (DCM)</td>
			<td>Fisher Scientific</td>
			<td>D/1857/17</td>
			<td>[75-09-2] 
			HPLC grade, unstabilised</td>
		</tr>
		<tr>
			<td>Dimethylformamide (DMF)</td>
			<td>Alfa Aesar</td>
			<td>22915</td>
			<td>[68-12-2] very toxic 
			HPLC grade 99+% pure</td>
		</tr>
		<tr>
			<td>Dimethylsulfoxide (DMSO)</td>
			<td>Alfa Aesar</td>
			<td>36480</td>
			<td>[67-68-5] very toxic 
			ACS, 99.9% min</td>
		</tr>
		<tr>
			<td>Cyclohexane</td>
			<td>Fisher Scientific</td>
			<td>C/8936/15</td>
			<td>[110-82-7] 
			HPLC grade, 99.8+%</td>
		</tr>
		<tr>
			<td>Toluene</td>
			<td>Fisher Scientific Ltd</td>
			<td>T/2306/15</td>
			<td>[108-88-3] 
			HPLC grade</td>
		</tr>
		<tr>
			<td>Benzene</td>
			<td>Sigma Aldrich</td>
			<td>401765</td>
			<td>[71-43-2] 
			puriss pa reagent</td>
		</tr>
		<tr>
			<td>5 -120 mL automatic pipette</td>
			<td>Sartorius</td>
			<td>Picus eLine</td>
			<td>systematic error in specification: 
			for 120mL is &#177;0.48 mL, 
			for 60 mL is &#177;0.36 mL, 
			for 12 mL is &#177;0.24 mL</td>
		</tr>
		<tr>
			<td>VIAL screw clear 1.5ml + CAP bakelite solid screw PTFE lined for 10mm vial</td>
			<td>Jaytee Biosciences</td>
			<td>JW41110 + 
			JW43927</td>
			<td>Capped vial used for validating accuracy and precision of dispensed solvent</td>
		</tr>
		<tr>
			<td>Crystal Structural Database</td>
			<td>The Cambridge Crystallogra-phic Data Centre (CCDC)</td>
			<td>Cambridge Structural Database (CSD)</td>
			<td>Containing over 900,000 entries from x-ray and neutron diffraction analyses</td>
		</tr>
		<tr>
			<td>powder X-ray diffractometer</td>
			<td>Panalytical</td>
			<td>X-Pert PRO MPD</td>
			<td>Equipped with an X&#8217;Celerator detector with Cu K&#945; radiation</td>
		</tr>
		<tr>
			<td>powder X-ray diffractometer data Collector software</td>
			<td>Panalytical</td>
			<td>X&#8217;Pert HighScore Plus v3.0</td>
			<td>solftware package used to adquire the PXRD data</td>
		</tr>
		<tr>
			<td>Rietveld refinement software including Scherrer equation</td>
			<td>BRUKER</td>
			<td>Version 6 of TOPAS-Academic</td>
			<td>To prepare phase composition and crystal size from PXRD scans</td>
		</tr>
		<tr>
			<td>HPLC equipment</td>
			<td>Agilent</td>
			<td>HP1200 Series modular HPLC system</td>
			<td>HPLC high pressure binary pump, autosampler, Peltier type column oven with 6 &#181;L heat exchanger and Diode Array Detector with a semi-micro flow cell (1.6uL, 6mm pathlength).</td>
		</tr>
		<tr>
			<td>HPLC column</td>
			<td>Agilent</td>
			<td>1.8mm Zorbax XDB C18,</td>
			<td>(4.6mm ID &#215; 50 mm length)</td>
		</tr>
		<tr>
			<td>Ball mill grinder</td>
			<td>Retsch</td>
			<td>MM400</td>
			<td>modified: replaced safety cover for external safety screen</td>
		</tr>
		<tr>
			<td>14 mL snap closure stainless steel jars</td>
			<td>In house</td>
			<td></td>
			<td>manuctured from 316 stainless steel</td>
		</tr>
		<tr>
			<td>14 mL screw closure stainless steel jars</td>
			<td>In house</td>
			<td></td>
			<td>manuctured from 316 stainless steel - 
			contains a PTFE washer</td>
		</tr>
		<tr>
			<td>Stainless steel ball bearings:</td>
			<td>Dejay Distribution Ltd</td>
			<td>7.0 mm (1.37g)</td>
			<td>Stainless Steel Balls A.I.S.I. 420 Carbon (0.25/0.35%) &#38; Chromium (12/14%)</td>
		</tr>
		<tr>
			<td>&#34;Push a Button&#34; software</td>
			<td>Developed at Department of Chemistry</td>
			<td></td>
			<td>Written in Visual Basic. It activates an electronically controlled switch (relay).</td>
		</tr>
		<tr>
			<td>&#34;Push a Button&#34; Solenoid</td>
			<td>Magnet Schultz</td>
			<td>Type 609RP 
			12 Volt DC</td>
			<td>609RP (RP stands for) 
			R - for spring-return 
			P - for push-rod</td>
		</tr>
		<tr>
			<td>&#34;Push a Button&#34; 
			Solenoid holder</td>
			<td>Department of Chemistry</td>
			<td></td>
			<td>To hold solenoid over START button on the MM400</td>
		</tr>
		<tr>
			<td>&#34;Push a Button&#34; Relay</td>
			<td>KM Tronic</td>
			<td>USB one relay</td>
			<td>USB Relay Controller - One Channel - HyperTerminal ASCII commands. Connection to a PC&#39;s USB port using VCP (Virtual COM port).</td>
		</tr>
		<tr>
			<td>re-usable adhesive putty</td>
			<td>Bostik</td>
			<td>Blu-Tack</td>
			<td>Used to hold the jar fixed on the bench.</td>
		</tr>
	</tbody>
</table>

reliable mechanochemistry: protocols for reproducible outcomes of neat and liquid assisted ball-mill grinding experiments

Итоги равновесия шарика мельница измельчения может кардинально изменить как функция даже крошечные различия в экспериментальных условиях, таких как наличие очень небольшое количество растворителя добавлен. Можно воспроизвести и точно захватить это чувствительность, экспериментатор должен внимательно рассмотреть каждый единственный фактор, который может повлиять на шаровой мельнице измельчения реакции под следствием, от обеспечения размольных чистой и сухой перед использованием, чтобы точно Добавление стехиометрии исходных материалов, для проверки что поставка растворителей тома точной, чтобы обеспечить, что взаимодействие между растворителем и порошок хорошо понимали и, при необходимости, добавляется определенное время замачивания к процедуре. Предварительные кинетические исследования необходимы для определения необходимости фрезерования времени для достижения равновесия. Только тогда можно получить изысканный фазы состав кривых как функция концентрации растворителя под мяч мельница жидкости помощь шлифовальные (ЗАПАЗДЫВАНИЕ). С помощью строгого и тщательного процедур, аналогичных тем, которые здесь представлены, можно получить такое фрезерование равновесия кривых для практически всех фрезерных систем. Система, которую мы используем, чтобы продемонстрировать эти процедуры – это реакция обмен дисульфида, начиная от эквимолярных смесь двух homodimers для получения на количественных гетеродимера равновесия. Последняя образуется шаровая мельница помола как два разных полиморф, Форма A и B формы. Отношение R = [Форма B] / ([Форма A] + [Форма B]) при фрезеровании равновесия зависит от природы и концентрацию растворителя в банку, фрезерование.

Этот протокол всегда запускается экспериментатор проверка его или ее дозирования навыки и проверки на качество и производительность пипетки или шприцы используются. Лучше всего это делается путем выполнения учебных комплектов на дозирования точных объемов конкрет?...

Watch this Scientific Journal Video about Reliable Mechanochemistry: Protocols for Reproducible Outcomes of Neat and Liquid Assisted Ball-mill Grinding Experiments at JoVE.com

Reliable Mechanochemistry: Protocols for Reproducible Outcomes of Neat and Liquid Assisted Ball-mill Grinding Experiments

Мы представляем подробные процедуры для получения экспериментальных равновесия кривых фазового состава как функции растворителя концентрации в твердом состоянии системы под фрезерные условий.

Надежные механохимии: Протоколы для воспроизводимых результатов аккуратные и жидкости помощь шар мельница помола эксперименты

The equilibrium outcomes of ball mill grinding can dramatically change as a function of even tiny variations in the experimental conditions such as the ...

Research

JoVE Journal

Chemistry

Microwave-assisted Functionalization of Poly(ethylene glycol) and On-resin Peptides for Use in Chain Polymerizations and Hydrogel Formation

Microwave-assisted Functionalization of Polyethylene glycol and On-resin Peptides for Use in Chain Polymerizations and Hydrogel Formation

Микроволновая печь-помощь Функционализация поли (этиленгликоль) и On-смолы пептиды для использования в цепных полимеризации и гидрогеля формирования

One of the main benefits to using poly(ethylene glycol) (PEG) macromers in hydrogel formation is synthetic versatility. The ability to draw from a large ...

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Подготовка Silica наночастиц Через СВЧ-помощь кислотно-катализа

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

Conducting Miller-Urey Experiments

Проведение Миллер-Юри эксперименты

In 1953, Stanley Miller reported the production of biomolecules from simple gaseous starting materials, using an apparatus constructed to simulate the ...

Isolation and Preparation of Bacterial Cell Walls for Compositional Analysis by Ultra Performance Liquid Chromatography

Изоляция и подготовка бактериальных клеточных стенок для композиционного анализа с помощью ультра производительности жидкой хроматографии

The bacterial cell wall is critical for the determination of cell shape during growth and division, and maintains the mechanical integrity of cells in the ...

Post Column Derivatization Using Reaction Flow High Performance Liquid Chromatography Columns

Сообщение Колонка дериватизации с использованием реакции потока высокоэффективной жидкостной хроматографии Колонки

A protocol for the use of reaction flow high performance liquid chromatography columns for methods employing post column derivatization (PCD) is ...

CN-GELFrEE - Clear Native Gel-eluted Liquid Fraction Entrapment Electrophoresis

CN-GELFrEE - Clear Native гель-элюированный жидкая фракция Entrapment электрофорез

Protein complexes perform an array of crucial cellular functions. Elucidating their non-covalent interactions and dynamics is paramount for understanding ...

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC)

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography HPLC

Прямолинейный метод глюкозинолатов экстракции и анализа с высоким давлением жидкостной хроматографии (ВЭЖХ)

Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil ...

Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles

Жидкости клеточной просвечивающей электронной микроскопии для отслеживания самостоятельной сборки наночастиц

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully ...

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites

Удобный метод для извлечения и анализа с высокого давления жидкостной хроматографии и их метаболитов катехоламинов нейротрансмиттеров

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and ...

Total Internal Reflection Absorption Spectroscopy (TIRAS) for the Detection of Solvated Electrons at a Plasma-liquid Interface

Total Internal Reflection Absorption Spectroscopy TIRAS for the Detection of Solvated Electrons at a Plasma-liquid Interface

Полное внутреннее отражение абсорбционная спектроскопия (Тирас) для обнаружения сольватированного электронов в плазме жидкость интерфейс

The total internal reflection absorption spectroscopy (TIRAS) method presented in this article uses an inexpensive diode laser to detect solvated ...