Operation Manual ® Syncore Accessories 093013 en
Syncore® Accessories Table of contents Table of contents Read this operation manual through carefully before starting to use the BUCHI Syncore Product Line. Always keep these instructions ready at hand close to the equipment so that they may be consulted quickly at all times. Chapter 2 provides important safety instructions that must be followed to ensure safe operation of the unit. We reserve the right to make technical changes without prior notice.
Syncore® Accessories 1 Scope of delivery 1 Scope of delivery 1.1 Racks Crystal Rack R-4 Order Code 1 Rack R-4 for working volume of up to 4 x 500ml, incl. 4 glasses R-4 47790 Crystal Rack R-4 Analyst 1 Rack R-4 with cooling of the residual volu me for working volume of up to 4 x 500ml (tubes not included) 47794 Crystal Rack R-6 1 Rack R-6 for working volume of up to 6 x 500ml, incl.
Syncore® Accessories 1 Scope of delivery 1.2 Glass tubes and holders Order code Vessels R-4 without residual volume (Ø: 85 mm / H: 185 mm / Vol.: 500 ml) 1 Set of 4 vessels 38487 Vessels R-4 with residual volume (Analyst) (Ø: 85 mm / H: 205 mm / Vol.: 500 ml) 1 Set of 4 vessels, residual volume 3ml 47797 1 Set of 4 vessels, residual volume 1ml 47798 1 Set of 4 vessels, residual volume 0.3ml 47799 1 Set of 4 grad. vessels, residual vol. 3ml 47740 1 Set of 4 grad. vessels, residual vol.
1 Scope of delivery Syncore® Accessories Vessels R-12 without residual volume (Polyvap) (Ø: 48 mm / H: 147 mm / Vol.: 120 ml) 1 Set of 12 vessels for Rack R-12 Polyvap 40907 Vessels R-12 with residual vol., no graduation (Ø: 48 mm / H: 170 mm / Vol.: 120 ml) 1 glass, residual volume 3ml 46010 1 glass, residual volume 1ml 46011 1 glass, residual volume 0.
Syncore® Accessories 1 Scope of delivery 1.
Syncore® Accessories 1 Scope of delivery 1.5 Insulation for high boiling solvents 41922 Insulation for high boiler to Rack R-24 Consisting of: 1 Insulation plate, upper, R-24 41885 1 Glass insulation, R-24 and R-48 41887 1 Vacuum hose made of PFA ribbed, 0.
Syncore® Accessories 1 Scope of delivery 1.7 Low temperature insulation Insulation to Rack R-24 and Rack R-96, cpl. 1 Insulation complete to Rack R-24 and Rack R-96 38144 Figure 10: Low temperature insulation 1.
1 Scope of delivery Syncore® Accessories Inert gas cover R-24 41918 Consisting of: 1 Vacuum cover, no glass plate 1 Inert gas module Inert gas cover R-48 42860 Consisting of:. 1 Vacuum cover, no glass plate: 1 Inert gas module Figure 13: Inert gas cover complete 1.9 Flushback Module for Syncore Analyst R-6 & R-12 Flushback Module R-6, cpl. 48654 Constisting of: 1 Flushback Module R-6 2 Silicon tubes, 2 m 43094 4 Cabel binders Flushback Module R-12, cpl.
Syncore® Accessories 2 Safety 2 Safety This unit and all its components have been built in accordance with the state of the art and recognized safety rules. Nevertheless, certain risks and dangers may be involved when working with the unit or its individual components: • Whenever the unit is not being used in accordance with its intended purpose, or • Whenever the staff operating the unit have not lack sufficient training and know-how. 2.
2 Safety Syncore® Accessories Syncore Polyvap/Syncore single platform with accessories: • Parallel evaporation of solvents in various formats and containers across a range of temperatures from room temperature up to + 150 °C and within a range of pressures from 1 mbar up to ambient pressure.
Syncore® Accessories 2 Safety 2.5 Basic hazards The basic hazards arise from: • Chemicals that are toxic or cause allergic reactions, or can, in a chemical reaction, produce compounds that are toxic or cause allergic reactions. • Solvent materials which can form peroxides. • Very hot or very cold parts made of plastics and metals (Burn injuries). • Kinked hoses or the dissolving of hose materials used to introduce liquids, compressed gases under pressure.
2 Safety Syncore® Accessories 2.7 Modifications No modifications may be made on this unit or on spare and accessory parts, nor is use of spare or accessory parts other than those indicated in this Operation Manual permissible, without the prior written approval of BÜCHI Labortechnik AG. 2.8 Safety instructions Chemicals and solvents The unit must be clean before being operated. Residues of chemicals are to be removed following the general rules for working with chemicals.
3 Function,putting into operation, operation and maintenace Syncore® Accessories 3 Function, putting into operation operation and maintenance 3.1 Syncore Product Line Accessories The Syncore product line is modular throughout. Every accessory is usable at any time with a Syncore single platform and with all standard configurations. 3.2 The condenser unit Introduction The condenser unit is used to condense out solvent vapors under a reduced pressure and to collect them in a receiving flask.
Function,putting into operation, operation and maintenace Syncore® Accessories • Fasten the cold water supply to the connection units a and b using GL14 screwed fittings • Join the connection element c to the valve unit by means of a GL 14 sealing cap d. Figure 16: Cooler coonections Temperature of the cooling medium The temperature of the cooling medium significantly affects the condensation of the solvent vapors.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace 3.3 Racks Introduction The Syncore product line allows various racks to be used on a given platform. These permit the parallel processing of ... • in synthesis: 24 and 96 samples with working volum ranging from 1 to 40ml • in evaporation: 4 to 96 samples with working volume ranging from 1 to 500ml • in concentration: 4 to 12 samples with a working volume of up to 500ml resp.
Syncore® Accessories Function,putting into operation, operation and maintenace Sample volume (SV) Rack Minimum SV Optimum SV R-4 50 ml 500 ml R-4 with residual vol. 50 ml 500 ml R-6 25 ml 250 ml R-6 with residual vol. 25 ml 250 ml R-12 10 ml 120 ml R-12 with residual vol. 10 ml 120 ml R-24 5 ml 30 ml R-48 1 ml 20 ml R-96 0.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Use only clean distilled water. Whenever the racks are not going to be used for a prolonged time, empty them so as to keep deposits from forming on the metal shell. Syncore Analyst appendix sleeves To improve the ability to reach the final volume within the entire rack (faster and more stable), the appendix sleeve is used. It can be inserted into each Analyst rack position by means of the special tool.
Syncore® Accessories Function,putting into operation, operation and maintenace Empty positions Due to active cooling of the residual volume appendages on the glasses in the Rack R-6 with cooling of the residual volume, the rack should never be operated with some of the glasses empty without first sealing off the empty positions in the vacuum connection with plastic plugs. The cooling produces a cool condensation zone for solvents that evaporate out of glasses that are filled.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Rack R-12 Rack R-12 provides for the heating or cooling of test vessels with rounded bases. Only those glass vessels described in these Operating Instructions should be used. Retaining clamps In all the positions within the racks, the glass vessels are secured by retaining clamps a in the wall of the rack and - in order to obtain an optimal transfer of heat - are pressed against the metal surface. By adding approx.
Function,putting into operation, operation and maintenace Syncore® Accessories Customer-specific racks It is possible to build a customer-specific rack with various glass geometries and sizes.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace 3.4 Vacuum covers d c Figure 23: Vacuum Cover Introduction The vacuum connection is used in conjunction with a suitable vacuum source in order to place the sample tubes in a rack under a vacuum. For this reason, the vacuum connection is connected to the vacuum source by a cooling unit, then positioned against the test vessels in the rack and, finally, screwed down.
Function,putting into operation, operation and maintenace Syncore® Accessories Electrical connection Connect the plug a on the electrical cable of the vacuum connection to the 24 V connection socket b on the right side of the single platform. b a Figure 24: 24 V connection on the vacuum connection Warning: Under no conditions is it permissible to plug the plug into the socket if solvents or chemicals have flowed into the socket.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace To ensure a quick warming of the vacuum connection, the vortex drive should not be switched ON. A flashing in the display „Actual“ indicates that the heater for the vacuum connection is ON. This display keeps flashing until the setpoint temperature for the vacuum connection has been reached. As soon as the „Start“ button is activated, the display stays lit with a constant light.
Function,putting into operation, operation and maintenace Syncore® Accessories Glass plate The glass plate lets the operator observe the vacuum zone inside the vacuum connection. The operator can at all times see any spraying in one of the positions or any condensation that is occurring. A vacuum connection must never be used if the glass has been damaged. Glass plates that are cracked or whose edges have splintered off could shatter under the vacuum and cause material damage and personal injuries.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Maintenance of the vacuum connection The gas plates of the vacuum connections can be removed by releasing the two clamping screws a. For this reason, the “PEEK”-screws for the glass vessel seals must be tightened with the Syncore Universal Key (see section “Spare Parts”). a Figure 29: Releasing the screws of the vacuum connection Use a sponge dampened in alcohol to clean the coated plate of the vacuum connections.
Syncore® Accessories Function,putting into operation, operation and maintenace 3.5 Cooling plate c Introduction The cooling plate b is installed between the base plate a of the unit and a rack c. When used with a cooling aggregate and a valve, the cooling plate allows controlled cooling of a rack within a range from room temperature down to -20°C. b a When a valve is used, a rack can also be through the cooling plate, enabling operation with complex time / temperature profiles.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Then screw the holding clamps onto the cooling plate. A Rack can now be put on, just as on the base plate. Figure 33: Fastening the cooling plate in position (2) It is important that the holding clamps be screwed on tightly. If not fastened adequately, the holding clamps do not hold the racks tightly enough to the cooling plate, which can lead to material damage and personal injuries.
Syncore® Accessories Function,putting into operation, operation and maintenace 3.6 Valves For all types of valves: Always secure the connections! Poorly secured hose connections can resullt in material damage and personal injuries. b Valve, 24 V DC to - 20°C, with hose nipples The temperature-controlled valve a is located between the cooling aggregate and the cooling plate. It controls the (temperature-dependent) flow of coolant into the cooling plate.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace 3.7 Inert gas cover / inert gas module Using the inert gas cover, 24 reaction glass vessels can be simultaneously sealed against the environmental temperature and they can be gassed with an inert gas. As a result, 24 chemical reactions can be carried out at the same time under inert gas (for example water exclusion via Argon).
Syncore® Accessories Function,putting into operation, operation and maintenace Function test Tightness Tightness is tested at slight gas excess pressure. a b c e Figure 38: Gas flow and bubble counter d To do so, the vacuum connection must be sealed with the SVL22 lid. The inert gas cover (or the inert gas module in connection with a vacuum cover) is placed onto the 24 test tubes in rack R-24. The inert gas cover is fastened to the test tubes using the two tightening nuts (safety screws).
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Working under inert gas Inert gas connection Valve Unit Vacuum Controller Cooling Unit a Inlet b Outlet Gas washing bottle Inert gas module Receiving flask Reflux module/ Rack R-24 Legend ------- Electrical connections Vacuum connections Inert gas connections ⊗ Valve or clamping buckles Figure 39: Hose coupling diagram For sensitive reactions where traces of steam or other gases can cause disturbances, we recomm
Function,putting into operation, operation and maintenace Syncore® Accessories Direct concentration We recommend direct concentration of reaction mixtures for sensitive reaction products, which are further processed directly in the same size (without transfer into another vessel). If you directly evaporate after a parallel reaction, the following procedure is used after the reaction: • Inert gas supply and discharge is interrupted (for example via hose clamps or by using a three-way cock).
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Maintenance of the intert gas module You can use organic solvents like ethanol or acetone to remove organic residues. You can use mild detergents and a soft (plastic) brush to clean the module. Punctured septa a can be removed by loosening the screws b, and individually replaced by new septa. You should visually inspect the septa after every reaction for damages and contamination.
Function,putting into operation, operation and maintenace Syncore® Accessories 3.8 Reflux module/flushback module The reflux module/flushback module a enables simultaneous condensation of solvent vapor in glass vessels b (= reflux*) via contact of the glass vessels with actively cooled metal ring, which surrounds each glass vessel.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Setting up Among others, the reflux module/flushback module consists of two metal plates with recesses for the individual test tubes. The two metal plates can be pushed against one another. They hold the test tubes via horizontal shear action and cool the test tubes in a defined zone through contact with an actively cooled metallic surface.
Syncore® Accessories Function,putting into operation, operation and maintenace Temperature of the cooling medium The ideal choice of the coolant temperature is depending on the boling point of the solvent, the reagents, and the set temperature on the rack heater. Wrong (too high) temperature of the reflux module/flushback module or the cooling medium can lead to loss of solvent or volatile reagents through the inert gas flow.
Syncore® Accessories 3 Function,putting into operation, operation and maintenace Removing the reflux/flushback module You can only remove the reflux/flushback module from the rack, after you have turned off the shaking motion. Before shaking motion of the Syncore basic unit stops, you must make sure that the temperature of the samples is clearly below the lowest boiling point of the solvents/reagents used.
Syncore® Accessories 4 Replacement Parts 4 Replacement parts Only original accessory and spare parts ensure operating safety and the proper functioning of this unit and its accessories in the Syncore line of equipment. The use of spare parts and accessories other than those from BUCHI is permissible only with prior approval from BÜCHI AG. 4.
Syncore® Accessories 4 Replacement Parts Rack R-48 and R-96 1 Set of 100 balancing springs 40765 1 Threaded Rack bar 40934 4.2 Glass tubes and holders Order code Vessels R-4 without residual volume (Ø: 85 mm / H: 185 mm / Vol.: 500 ml) 1 Set of 4 vessels 40765 Figure 48: Replacement parts, Rack R-48 and R-96 38487 Vessels R-4 with residual volume (Analyst) (Ø: 85 mm / H: 205 mm / Vol.
Syncore® Accessories 4 Replacement Parts Holder for R-6 vessels (Analyst or Polyvap) 1H older for 6 Syncore Analyst or Polyvap vessels 38483 Vessels R-12 without residual volume (Polyvap) (Ø: 48 mm / H: 174 mm / Vol.: 120 ml) 1 Set of 12 vessels for Rack R-12 Polyvap 40907 Vessels R-12 with residual vol., no graduation (Ø: 48 mm / H: 170 mm / Vol.: 120 ml) Figure 51: Holder for vessels R-6 1 vessel, residual volume 3ml 46010 1 vessel, residual volume 1ml 46011 1 vessel, residual volume 0.
Syncore® Accessories 4 Replacement Parts 4.
Syncore® Accessories 4 Replacement Parts Vacuum cover R-12 40909 40906 40905 Figure 57: Replacement parts, vacuum cover R-12 38272 38178 40915 Order code 1 Nut (for securing the glass plate to the vacuum cover) 38178 1 Set of sealing washers, PTFE-coated 2 units 40906 1 Set of support discs for the vacuum cover R-12, 12 units 40905 1 Set of PEEK bolt caps, 2 units 40909 1 Glass plate for vacuum cover R-12 40915 1 Sealing ring for glass plate R-6, R-12, R-24, R-48, R-96 40873 1 Set
4 Replacement Parts Syncore® Accessories Vacuum cover R-48 38495 38490 41838 Order code 1 Nut for securing the glass plate to the vacuum cover 38178 1 Set of 50 sealing washers PE 46591 1 Set of 12 PEEK screws 46592 1 Glass plate for the vacuum cover R-48 38428 1 Sealing ring for glass plate R-6, R-12, R-24, R-48, R-96 40873 1 Set of 50 plastic stoppers for R-48, R-96 40193 1 Set of 2 seals for PFA vacuum hose.
Syncore® Accessories 4 Replacement Parts 4.
Syncore® Accessories 33478 37693 4 Replacement Parts 25022 (1l) 40775 (2l) 40776 37695 05155 37694 37686 27344 03275 Figure 64: Condenser unit C Condenser unit C complete (PLASTIC + GLAS) Order code 1 Condenser unit C complete, 1 Liter, (PLASTIC+GLAS coated) 38371 Consisting of 1 Support rail for attaching the Condenser unit 37693 1 Cold trap, complete 33478 1 screw cap GL-14 cpl.
Syncore® Accessories 4 Replacement Parts 4.
Syncore® Accessories 4 Replacement Parts 4.7 Hoses Components Order code 1 Vacuum hose to vacuum cover length: 1m 26096 1 Water hose, length: 1m (for the cooling of the condenser unit or the Racks with residual volume) 04133 Quick coupling set (2 pcs) 42885 4.
Syncore® Accessories 5 Appendix 5 Appendix 5.1 Technical data Connection to inert gas module cpl., vacuum connection 24 V Power take-up for the vacuum connection 120 W max Ambient temperature 5°C-40°C Maximal gas overpressure 10 mbar Temperature range, vacuum connection Room temperature up to +70°C Description 5.
Syncore® Accessories 5 Appendix 5.3 Table of solvents Starting pressure to reduce the boiling point to 40 °C Solvent Formula Molecular weight in g/mol C2H4O2 60.0 695 Aceton C3H6O 58.1 n-Amylalcohol, n-Pentanol C5H12O 88.1 Acetic acid Energie of eva- Boiling point in poration in J/g °C at 1013 mbar Tightness in g/cm3 Vacuum in mbar for boiling at 40°C 118 1.049 44 553 56 0.790 556 595 37 0.814 11 C6H6 78.1 548 80 0.877 236 n-Butanol, tert. Butanol C4H10O 74.
5 Appendix Syncore® Accessories Resistance of polyethylene sealing discs Solvent A: Very good resistance: Sealing discs of PE (polyethylene) may be used without restrictions Acetaldehyde A Acetone A Benzene B Butanol A Chloroform C Diethyl ether B Dimethylformamide A Dimethylbenzene (Xylol) B Dioxane A Acetic acid A Acetic acid anhydride A Ethanol A Ethyl acetate A Hexane A Isobutanol A Isopropanol A Methanol A Methylene chloride B Nitrobenzene A Phenol A Propano
Syncore® Accessories 5 Appendix Resistance of FPM Solvent A: Very good resistance: FPM may be used without restrictions Acetaldehyde D Acetone D Benzene B Butanol A Chloroform B Diethyl ether D C: Poor resistance: Sealing deform. The sealings of FPM should be used only to a limited extent. We recommend that the sealings be tested beforehand (softening or wetting the sealing discs).
5 Appendix Syncore® Accessories Resistance of EPDM Solvent A: Very good resistance:EPDM may be used without restrictions Acetaldehyde B Acetone A Benzene D Butanol B Chloroform D Diethyl ether C C: Poor resistance: Sealing deform. The sealings of EPDM should be used only to a limited extent. We recommend that the sealings be tested beforehand (softening or wetting the sealing discs).
5 Appendix Syncore® Accessories Resistance of the perfluorelastomer sealings Solvent A: Very good resistance: Perfluorelastomer may be used without restrictions Acetaldehyde B Acetone A Benzene A Butanol A Chloroform A Diethyl ether A C: Poor resistance: Sealing deform. The sealings of Perfluorelastomer should be used only to a limited extent. We recommend that the sealings be tested beforehand (softening or wetting the sealing discs).
5 Appendix Resistance of PEEK Syncore® Accessories Solvent Resistance Acetaldehyde A A: Very good resistance: PEEK may be used without restrictions Acetone A Benzene A B: Moderate resistance: PEEK may swell. PEEK may generally be used, but may under some circumstances have to be replaced after being used several times. Butanol A Chloroform A Diethyl ether A C: Poor resistance: PEEK deform. PEEK should be used only to a limited extent.
Syncore® Accessories 5 Appendix 5.4 FFC requirements (for USA and Canada) English: This equipment has been tested and found to comply with the limits for a Class A digital device, pusuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment.
5 Appendix Syncore® Accessories 5.
BÜCHI Labortechnik AG CH-9230 Flawil 1 / Switzerland T +41 71 394 63 63 F +41 71 394 65 65 www.buchi.
