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Knauer AZURA SMB Pilot Instructions Manual

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Document no. V6675

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Summary of Contents for Knauer AZURA SMB Pilot

  • Page 1 SMB systems Instructions Document no. V6675...
  • Page 2 For latest version of the siinstructions, check our website: https://www.knauer.net/en/Support/User-manuals Copyright: This document contains confidential information and may not be reproduced without written content of KNAUER Wissenschaftliche Geräte GmbH. © KNAUER Wissenschaftliche Geräte GmbH 2019 All rights reserved. AZURA® is a registered trademark of KNAUER Wissenschaftliche Geräte GmbH.

  • Page 3: Table Of Contents

    AZURA SMB Pilot System ........
  • Page 4 Table of contents 7. Start-up ................24 Initial start-up checklist .
  • Page 5 Table of contents 12. Technical data ..............46 12.1 General system parameters .

  • Page 6: Product Information

    Product information 1. Product information 1.1 Intended use Note: Only use the system for applications that fall within the range of the intended use. Otherwise, the protective and safety equipment of the system could fail. Application Separation and extraction Pharmaceutical chemistry Chiral compound (cis-trans phytol, stero- ids, peptides, antibiotics, etc.) Food chemistry...

  • Page 7: Azura® Smb Pilot

    Product information 1.2.2 AZURA® SMB Pilot The AZURA® SMB Pilot is designed for the separation of binary mixtures on a hundred gram to kilogram scale and is typically used with columns up to 50 or 100 mm ID. Its special emphasis is put on the continuous ope- ration mode and highest productivity.

  • Page 8: Azura® Smb Lab

    feed pump inlet is not connected to a multi- position valve. Product information Feed Raffi nate Zone 3 Column Zone 2 Zone 4 switching direction Zone 1 Extract Eluent Schematic AZURA® SMB design Fig. 3 SMB design scheme KNAUER_Brosch_SMB_12do.indd 14 28.08.17 1 1.3.1 AZURA®...

  • Page 9: Simulated Moving Bed Principle

    Simulated Moving Bed principle 2. Simulated Moving Bed principle 2.1 Introduction Due to the fast development of new compounds and the more preci- se knowledge about them, there is an increasing demand for purified products. In most cases, chemical syntheses produce a lot of side com- ponents.
  • Page 10 Simulated Moving Bed principle interstitial velocity. At the time t a well defined amount of the sample mixture is injected into the column. Due to different interaction forces of the mixture components and the adsorbent (different migration ve- locities), a separation of the mixture into the pure components will take place.

  • Page 11: True Counter-Current Process

    Simulated Moving Bed principle into the pure components due to different interaction forces to the adsor- bent. The time between two pulses i and i+1 have to be chosen in such a case, that the slowest component of pulse i elutes before the fastest compo- nent of pulse i+1 or just before they overlap too much, where pulse i is injected before pulse i+1 (Fig.
  • Page 12 Simulated Moving Bed principle Unloaded solid (adsorbent) is continuously filled into the upper end of the column, while liquid (eluent) is pumped into the lower one. The bina- ry (or pseudo-binary) feed-mixture is continuously injected in the middle of the column. To separate the components of the mixture, they have to be differently adsorbed on the solid.

  • Page 13: Simulated Counter-Current Process

    Simulated Moving Bed principle 2.4 Simulated counter-current process The simulated counter-current process (Simulated Moving Bed - SMB) was developed in the early 60th by the Universal Oil Products Company. It was mainly applied to industrial-scale separations, like the xylene separation or the fructose-glucose separation.
  • Page 14 Simulated Moving Bed principle For SMB applications the large column in Fig. 8 can also be substituted by a number of chromatographic columns. This is sketched for 8 columns in Fig. 9. Like in the TMB process there are feed, eluent, extract and raffinate inlets and outlets, dividing the circle of columns into four sections.

  • Page 15: Efficiency And Economic Aspects

    Simulated Moving Bed principle In Fig. 10 the concentrations are normalized on the feed concentration of each component. These normalized concentrations are plotted versus the time coordinate. There are typical zigzag profiles, where a triangle sym- bolizes one switching interval or tact. After 12 of these intervals (i.e. 3 full cycles for a four column SMB process) the cyclic steady state is reached (two proceeding triangles are almost identical).

  • Page 16: Scope Of Delivery

    3. Scope of delivery Note: Only use original parts and accessories made by KNAUER or a com pany authorized by KNAUER. 3.1 AZURA SMB Lab System ƒ 1 x AZURA® Assistant ASM 2.1 L with 1 x AZURA® Pump P4.1S (10 ml pump head) and 1 x 8-Multiposition-valve ƒ...

  • Page 17: Azura Smb Pilot System

    Scope of delivery 3.2 AZURA SMB Pilot System ƒ 1 x AZURA® Assistant ASM 2.1 L with 1 x 8-Multiposition-valve ƒ 3 x AZURA® Assistant ASM 2.1 L with 2 x 8-Multiposition-valves ƒ 4 x AZURA® Pump P 2.1 L ƒ...

  • Page 18: Basic Safety Instructions

    ƒ Only use a given PEEK fitting for one specific port and never re-use it for other ports. Always install new PEEK fittings on each separate port. ƒ Follow KNAUER or manufacturer’s instructions on caring for the co- lums. AZURA® SMB system instructions V6775...

  • Page 19: Warning Notifications

    Take the device completely out of operation by disconnecting the power plug from the power supply (wall socket or power strip). Opening the device The device may be opened by the KNAUER Technical Support or any company authorized by KNAUER only. 4.4 Warning notifications Possible dangers related to the device are divided into personal and material damage in these instructions.

  • Page 20: Decontamination

    Decontamination Report Devices without a completed Decontamination Report will not be repai- red. If you would like to return a device to KNAUER, make sure to enclose a completed Decontamination Report with the device: https://www.knauer.net/decontamination-report.

  • Page 21: Unpacking And Setup

    Unpacking and setup 6. Unpacking and setup The HPLC system will be set up, installed and commissioned by KNAUER or a company authorized and contracted by KNAUER. Note: KNAUER recommends inviting future users to be present while set- ting up and commissioning the module so that they can become familiar with the analyzer and how to handle it.

  • Page 22: Earthquake Areas

    Unpacking and setup 6.1.3 Earthquake areas If you are located in an earthquake area, use the bore holes in the side panels to secure the device. The bore holes are located on either right or left side panel. 6.2 Storing unopened shipping boxes In your planning, include following information for immediate storage.

  • Page 23: Power Supply

    ƒ Beforehand, make sure to use power cables which are admitted for use in your country. ƒ Replace defective power cab les only with accessories from KNAUER. ƒ Do not replace detachable power cables with different cable types. Electronic defect Electronic hazard when using an identically constructed power adapter from another manufacturer.

  • Page 24: Flow Charts

    Unpacking and setup 6.6 Flow charts Fig. 11 Flow chart for AZURA® Lab system Fig. 12 Flow chart for AZURA® Pilot system AZURA® SMB system instructions V6775...

  • Page 25: Connecting System To Computer Via Lan

    6.7.1 Connecting the single devices to the computer Note: HPLC devices made by KNAUER work only with IP adresses which are assigned via IPv4. IPv6 is not supported. This section describes how to set up an HPLC system in a local area net- work (LAN) and how a network administrator can integrate this LAN into your company network.

  • Page 26: Configuring The Router

    6.7.4 Configuring the router The router is preset at the factory. You find information about IP address, user name and password in the router instructions: www.knauer.net/router Process Steps 1. To open the router configuration, start your Internet browser and enter the IP address (not valid for all routers).

  • Page 27: Controlling Several Systems Separately In A Lan

    Unpacking and setup 6.7.6 Controlling several systems separately in a LAN Devices connected to a LAN communicate through ports, which are part of the IP address. If more than one HPLC system is connected to the same LAN and you plan on controlling them separately, you can use different ports to avoid interference.
  • Page 28 Unpacking and setup Electronic defect Connecting cables to the multi-pin connector of a switched on device cau ses a short circuit. Turn off the device before connecting cables. Pull the power plug. Electronic defect Electrostatic discharge can destroy the electronics. Wear a protective bracelet against electrostatic discharge and ground.

  • Page 29: Start-Up

    ƒ Devices are positioned in the correct location. ƒ The power plugs are connected. ƒ The network connection to the router is established ƒ The chromatography software has been installed by KNAUER or a com pany authorized by KNAUER. ƒ The capillaries are connected.

  • Page 30: Shut Down

    Start-up Step Task Power up the router and wait until the self-test is performed. Power up all instruments and the PC. If a user management is used on the PC, login with the correct credentials. Start the PurityChrom® software with double click on the desk- top icon.

  • Page 31: Removing Air, Flushing/Cleaning The Smb And Cleaning Columns

    Start-up 7.3.1 Removing air, flushing/cleaning the SMB and cleaning columns To remove air from the SMB system, flush/clean the SMB or clean the columns, the system must be switched into the “Open Loop” mode. After- wards the pumps will be started step by step and the air or the contami- nation will be removed from the system.

  • Page 32: Flushing The System

    Start-up Step Task Set the flow rate at 10 % of the pump heads max. flow. Suck eluent through the pump. When no more air bubbles are visible in the inlet tubing, stop the pump and close the purge valve. 7.3.3 Flushing the system Note: For flushing the system without column, proceed here.

  • Page 33: Washing One Single Column

    Start-up Step Task Suck the eluent through the pump and wait until no more air bubbles leave the pump. Close the purge valve. Wait until there is a stable flow rate exiting the raffinate line and no more air bubbles are visible in the raffinate outlet. A slow dripping out of the waste line can occur.

  • Page 34: Flushing All Columns

    Start-up Step Task Set the valves “pump Zone 1 out” and “pump Zone 1 in” to the number of the column you want to clean up. Set every other column to +4 positions in comparison of the “washing column“. e.g.: washing of column 1 pump “Zone 1 out”...

  • Page 35: Operation

    Operation 8. Operation 8.1 Software operation To operate the system with software, you have to establish a connection between the LAN port and a computer. The system can be controlled with Puritychrom® MCC. You find a detailed description on chromatogra- phy software in the corres ponding software instructions (document no.

  • Page 36: Sop: Azura® Smb Separation

    Operation Color Status Operation flashes green The device not ready ƒ Wait until the device is rea- for operation. dy for operation. blue The device is in ƒ Press the standby button standby to end the standby. 8.3 SOP: AZURA® SMB separation For an overview of the flow scheme, refer to Fig.

  • Page 37: Pausing The Separation

    Operation Step Task Check for leakage and proper work of pumps and flowmeter. Check dripping at the Extract and Raffinate outlets. 8.3.3 Pausing the separation Step Task If required, the SMB system can be paused at every time by clicking the pause button ( The time will be paused, and all pumps will stop.

  • Page 38: Stopping The Separation

    PurityChrom® MCC is closed. Insert the following files into the described subdirectories: KNAUER-SMB-1-3-3-1.vis C:\PurityChrom\Visualisation\  Visualisation Files KNAUER SMB 1-3-3-1.bmp C:\PurityChrom\Visualisation\  Visualisation Backgrounds Start the PurityChrom® MCC Software. Change the start position of the valves according to Tab. 2. Valve Valve positions Tab.
  • Page 39 Operation Procedure Step Task Open the PurityChrom® MCC Setup here: Change the Startposition of Valve 1 to 1. Change the Startposition of Valve 2 to 1. Change the Startposition of Valve 3 to 2. AZURA® SMB system instructions V6775...
  • Page 40 Operation Step Task Change the Startposition of Valve 4 to 5. Use the arrow buttons to switch to the Valves 5 to 8. Change the Startposition of Valve 5 to 7. Change the Startposition of Valve 6 to 8. Change the Startposition of Valve 7 to 8. Close the Setup here: AZURA®...
  • Page 41 Save the current changes with <Ja>. Close the PurityChrom® MCC Software. Start the PurityChrom® MCC Software. Open the Visualisation here: Open the Visualisation Setup here: Load the Visualisation “KNAUER SMB 1-3-3-1”. Close the Visualisation Setup. AZURA® SMB system instructions V6775...

  • Page 42: From 2:2:2:2 To 1:1:1:1

    Operation Step Task The change to the zone configuration 1:3:3:1 is completed. You should see the following visualisation: 8.4.2 From 2:2:2:2 to 1:1:1:1 This section describes the change of the zone configuration to 1:1:1:1. Step Task Install one column on every second position: Column 1 at Position 1 Column 2 at Position 3 Column 3 at Position 5...

  • Page 43: Functionality Tests

    9.1 Installation Qualification (IQ) The customer may request the IQ of KNAUER devices which is free of charge. In case of a request, the Technical Support of KNAUER or from a provider authorized by KNAUER performs this functionality test during the installation.

  • Page 44: Troubleshooting

    Troubleshooting 10. Troubleshooting 10.1 First measures 1. Check all cabling. 2. Check all screw fittings. 3. Check whether air has gotten into the supply lines. 4. Check device for leaks. 5. Pay attention to system messages. 10.2 LAN Go through the following steps, in case no connection between the com- puter and the devices can be established.

  • Page 45: Possible Problems And Solutions

    Troubleshooting 10.3 Possible problems and solutions Note: If you have problems with the handling of a single device, please refer to the troubleshooting section of the respective instructions. Device/system Problem Solution SMB system During the procedure of the ƒ Switch the valve position until the initial valve position and flush the sop start up, the eluent exits system step by step according to...

  • Page 46: Maintenance And Care

    Maintenance and care 11. Maintenance and care 11.1 SOP: Cleaning procedure for pressure release valves and connected tubings for AZURA® Lab SMB Note: This procedure is valid for AZURA® Lab SMB A29001 only. 11.1.1 Zone 1 pump & zone 2 pump Follow this procedure to clean the pressure release valves and the con- nected tubings of zone 1 pump and zone 2 pump.

  • Page 47: Sop: Cleaning Procedure For Pressure Release Valves And Connected Tubings For Azura® Pilot Smb

    Maintenance and care Step Task Disconnect the tubing a on the t-cross 1 of each pump (see Fig. 13). Connect the tubing a with a coupling and close the open side of the coupling (1/16”) with a blind fitting. Close the open position on the t-cross 1 with a blind fitting Turn on the feed pump and set the flow rate to 80 % max.

  • Page 48: Maintaining The Azura® Lab System

    4 pump) Suggest maintenance interval pumps: Please refer to the Service Manual of the pump (document no. V6875A, available on Partner Area of KNAUER website, only for trained service technicians). Spare parts for pump heads: Please refer to the Service Manual for pump heads (document no.

  • Page 49: Decommissioning

    Maintenance and care 11.5 Decommissioning Auxiliary material The system is designed for the use of different solvents. In case the system has not been used for several weeks, solvent residues may cause damage. We, therefore, recommend to: ƒ Flush the capillaries. ƒ...

  • Page 50: Transport

    11.6 Transport Carefully prepare the device for transport. If you want to return your device to KNAUER for repairs, enclose the Service Request Form which can be downloaded from our website. For a secure transport, note the weight and dimensions of the device (see chapter „Technical data“.

  • Page 51: Technical Data

    Technical data 12. Technical data 12.1 General system parameters Parameter AZURA® SMB Lab AZURA® SMB Pilot Max. flow rate * 50 ml/min 500 ml/min Recommended 2–28 ml/min 2–200 ml/min flow rate * Max. delivery 1880 psi / 130 bar / 1450 psi / 100 bar / pressure * 13 MPa...

  • Page 52: Wetted Materials

    Technical data 12.3 Wetted materials Valid for AZURA® SMB Lab system (Art. Nr. A29000 and A29001) and AZURA® SMB Pilot system (Art. Nr. A29501). Note: For chemical compatibility of wetted materials, see chapter 13 on page 48. The components of the SMB system contain the following wetted parts: Pumps Material Description...

  • Page 53: Chemical Compatibility Of Wetted Materials

    The following list contains information about the chemical compatibility of all wetted materials which are used in devices made by KNAUER. The data bases on a literature research on the manufacturer specifications of the materials. The wetted materials of the present device are listed in chapter “Technical data”.
  • Page 54 Chemical compatibility of wetted materials Polyimide (Vespel®) This material is wear-resistant and permanent resilient thermically (up to 200 °C) as well as mechanically. It is chemically broadly inert (pH range 1–10) and is especially resistant against acidic to neutral and organic sol- vents, but vulnerable to pH strong chemical or oxidizing environments: It is incompatible with concentrated mineral acids (such as sulfuric acid), glacial acetic acid, DMSO and THF.

  • Page 55: Non-Metals

    Chemical compatibility of wetted materials 13.3 Non-metals Diamond-like carbon (DLC) This material stands out due to its high hardness, low friction coefficient and thus minimum wear. In addition, it is highly biocompatible. DLC is inert against all acids, alkalis and solvents commonly used in HPLC. Ceramic Ceramic is resistant against corrosion and wear and is fully biocompati- ble.

  • Page 56: Metals

    Chemical compatibility of wetted materials 13.4 Metals Stainless steel Stainless steel is, apart from PEEK, the standard material in HPLC. Steels with WNr. 1.4404 (316L) are used, or a mixture with higher compatibility. They are inert against almost all solvents. Exceptions are biological appli- cations which are metal ion sensible, and applications with extreme corro- sive conditions.

  • Page 57: Legal Information

    A warranty seal is attached on some devices. The warranty seal is co- lor-coded. A blue seal is used by the assembly or technical support of KNAUER for devices to be sold. After repair, service technicians stick an orange seal in identical position. If unauthorized persons interfere with the device or the seal is damaged, the warranty claim becomes void.

  • Page 58: Disposal

    2001), old devices manufactured by KNAUER are marked as waste electri- cal and electronic equipment: 160214. WEEE registration KNAUER as a company is registered by the WEEE number DE 34642789 in the German „Elektroaltgeräteregister“ (EAR). The number belongs to category 8 and 9, which, among others, comprise laboratory equipment.

  • Page 59: Index

    Index 16. Index accessories 11 maintenance 41 application 1 operating environment 16 capillary 18 Operation Qualification (OQ). see functionality tests wetted materials 46 check valve 42, 43 power chemical compatibility 46 disconnecting 44 cleaning 26, 41 supply 18 column power-up 24 cleaning 26 pressure release valve 41 washing 29...
  • Page 60 Index technical data 45 technical parameters 45 terminal strip 22 test. see functionality tests transport 44 damage 51 troubleshooting 39 unpacking 17 valve VICI 42, 43 wetted materials 46 warranty conditions 51 warranty seal 51 wetted materials 45 chemical compatibility 46 zone configuration 33 AZURA®...
  • Page 61 Latest KNAUER instructions online: https://www.knauer.net/en/Support/User-manuals KNAUER Phone: +49 30 809727-0 Wissenschaftliche Geräte GmbH Fax: +49 30 8015010 Hegauer Weg 38 E-Mail: info@knauer.net 14163 Berlin Internet: www.knauer.net © KNAUER 2019...

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