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Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley,

Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 1 User Guide QuadraSilTM Metal Scavengers Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 2 User Guide - QuadraSilTM Metal Scavengers Contents Page Introduction 3 Product Availabilty 3 QuadraSilTM Range 4 Features and Appearance 4 Guidelines for Use 5 Metal-Contaminated Solutions 5 Metal Scavenging Applications 6 iron chloride 6 copper acetate 6 triphenylphosphinecobalt(III)chloride 7 copper acetylacetonate 7 palladium acetate 8 copper bromide 8 ROPACTM 9 silver acetate 10 Catalyst Scavenging Example Grubbs catalyst 10 Metal Recovery 11 Storage 11 Appendix: QuadraSilTM Selection Guide Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 3 User Guide - QuadraSilTM Metal Scavengers Introduction The QuadraSilTM range of metal scavengers offers an attractive solution to metal contamination problems associated with pharmaceutical and fine chemical processing complementing the QuadraPureTM scavenger resin range. The QuadraSil™ products are functionalized silicas specifically designed for extraction of metal contaminants from organic and aqueous systems. As with the QuadraPure™ range, the very low levels of extractable impurities make products particularly suitable for GMP-compliant applications in both batch and continuous processing. The QuadraSilTM series are ideal for use in R&D applications as they are extremely fast scavengers and easy to isolate by filtration. A QuadraSilTM metal selector guide is given in the Appendix. Reaxa is continually developing the applications of its metal scavengers. The Company can also offer expertise in using all its metal-scavenger products in flow. Customer support in helping solve problems across the chemical industry sectors is a particular strength. For further information please contact Reaxa at info@reaxa.com. microscope image of QuadraSil™ R&D quantities of QuadraPure™ and QuadraSil™ as well as test kits for screening are available from Sigma-Aldrich at: www.sigma-aldrich.com For technical support, bulk quotations and information please contact: info@reaxa.com Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 4 QuadraSilTM Range QuadraSil™ functional group mmol/g Aldrich order # AP NH2 amino propyl 2.0 679534 MP SH mercaptopropyl 1.2 679526 MTU NHMe S N H methylthiourea 1.4 679518 TA N H H N NH2 triamine 1.0 679496 Features and Appearance • functionalised spherical mesoporous silicas • compatible with organic, aqueous, protic and aprotic media • extremely fast scavenging • zero swelling characteristics ideal for use in fixed bed applications • surface area 715 m2/g • average particle size 54 µm • mechanically and thermally robust microscope images of QuadraSil™ highlighting the regularity of size and shape The QuadraSilTM particles are highly robust and chemically resistant free-flowing silicas. The narrow particle size distribution, highly spherical shape, and zero swell makes these products suitable for use in fixed bed and cartridge format. Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 5 Guidelines for Use Note: For further detailed user application notes, GMP regulatory support data, and advice on specific problems, please write to info@reaxa.com Metal-Contaminated Solutions: In metal contaminated organic solvents, direct addition of QuadraSilTM will effect scavenging. Typically, add 5 g per 100 ml metal-contaminated solution and leave to gently agitate at room temperature. Metal removal is often complete in five minutes and can frequently be observed by a colour change in both the scavenger and the solution (see below). The resin is simply removed by filtration. The rate of metal scavenging can be increased by the addition of more resin, raising the temperature or increasing the agitation rate. original TA MTU AP MP Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 6 QuadraSil™ Metal Scavenging Applications The following examples show simple trials for metal salt removal from common solvents. In each case the picture shows the original solution (far left) and then after treatment with the QuadraSil™ range at the loading recommended for initial testing (0.5 g per 10 ml). Times to clear the solution are recorded. Fe(III)Cl3 1000ppm solution of FeCl3 in THF – 100ml solution: 291mg FeCl3 in 100ml THF MP AP TA MTU Fe(III)Cl3 N/A < 2 min < 2 min < 2 min Cu(II)(OAc)2 1000ppm solution of Cu(OAc)2 in THF – 100ml solution: 258mg Cu(OAc)2 in 100ml THF MP AP TA MTU Cu(II)(OAc)2 < 2 min < 2 min 3 min 4 min Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 7 Co(II)Cl2(PPh3) 1000ppm solution CoCl2(PPh3) in THF – 100ml solution: 1100mg CoCl2(PPh3) in 100ml THF MP AP TA MTU Co(II) dichlorobis-TPP N/A < 2 min 6 min 3 min Cu(II)(acac)2 1000ppm solution Cu(acac)2 in THF – 100ml solution: 412mg Cu(acac)2 in 100ml THF MP AP TA MTU Cu(II)(acac)2 15 min N/A 8 min N/A Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 8 Pd(II)(OAc)2 1000ppm solution Pd(OAc)2 in DCM – 100ml solution: 213mg Pd(OAc)2 in 100ml DCM MP AP TA MTU Pd(II)(OAc)2 ~1 min ~1 min ~1 min ~1 min Cu(I)Br 1000ppm solution CuBr in THF – 100ml solution: 213mg CuBr in 100ml THF MP AP TA MTU Cu(I)Br < 2 min < 2 min < 2 min < 2 min Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 9 Rh(CO)(PPh3)(acac) 1000ppm solution Rh(CO)(PPh3)(acac) in DCM – 100ml solution: 481mg Rh(CO)(PPh3)(acac) in 100ml DCM MP AP TA MTU Rh(CO)(PPh3)(acac) < 5 min > 24 h > 24 h > 24 h Rh(CO)2(acac) 1000ppm solution Rh(CO)2(acac) in DCM – 100ml solution: 239mg Rh(CO)2(acac) in 100ml DCM MP AP TA MTU Rh(CO)2(acac) 2 min 2 min 2 min 2 min Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 10 Ag(I)(OAc) 1000ppm solution Ag(OAc) in THF – 100ml solution: 155mg Ag(OAc) in 100ml THF MP AP TA MTU Ag(I)(OAc) < 4 min 50 min N/A 40 min QuadraSil™ Catalyst Scavenging Example Removal of ruthenium following metathesis using the Grubb’s catalyst is a significant problem overcome by very few scavengers. The QuadraSil™ range, with AP in particular, show excellent scavenging ability for this catalyst. In the picture below the starting solution shown contains 595 ppm Ru. 5 ml aliquots were treated with 250 mg of each QuadraSil™. All reduced the levels to below 5 ppm, with QuadraSil™ AP clearing the solution in 1½ h. QuadraSil™ initial Ru (ppm) % Ru removal Time (h) AP 595 >99 1.5 MP 595 >99 <16 MTU 595 >99 <16 TA 595 >99 <16 original AP MP MTU TA Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 11 Metal Recovery Through Reaxa’s partnership with Umicore we are able to offer complete metal management solutions to our customers. Storage The QuadraSilTM range of products are air-stable and can be stored at room temperature. Reaxa QuadraSil TM User Guide November 2006 Reaxa Ltd, Hexagon Tower, Blackley, Manchester M9 8ZS, UK T: +44 (0)161 721 2202; F: +44 (0)161 721 2005; E: info@reaxa com; W: www reaxa com 12 APPENDIX QuadraSilTM Selection Guide Please note that the following is a guide only and based on trials performed at Reaxa together with customer feedback. The efficiency of a metal scavenger will depend upon a number of factors including the oxidation state of the metal involved, pH and potential competing complexation by other ligands present and/ or the solvent. It is recommended that a range of QuadraPureTM and QuadraSilTM are assayed for each metal contamination problem. MP AP TA MTU Fe(III) Cu(II) Cu(I) Co(II) Ni(II) Pd(II) Pt Ru(II) Rh(II) Ag(I) Excellent Scavenging Ability (>99% removal, under 10 min) Significant Scavenging Ability (>98% removal, up to 24 h) – Not Tested /No Significant Scavenging Ability uploads/Geographie/ quadrasil-metal-scavengers-user-guide.pdf