CryoFocus-4 GC Cryogenic Trap

CryoFocus-4 GC Cryogenic Trap Installation Guide CryoFocus-4 onto Shimadzu GC-2010 www.atasgl.com

Disclaimer ATAS GL International B.V. makes no representations or warranties with respect to the contents or use of this manual and specifically disclaims any express or implied warranties of merchantability or fitness for any particular purpose. Further ATAS GL International B.V. reserves the right to revise this manual and to make changes to its content at any time, without obligation to notify any person or entity of such revisions or changes. The instruments are similarly subject to change without notice. Copyright No part of this manual may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopying and recording, for any purpose other than the purchaser's personal use without the written consent of the copyright holder. ATAS GL International B.V., 2011-2012 All rights reserved. ATAS GL International B.V. De Sleutel 9 5652 AS Eindhoven The Netherlands Telephone: +31 (0)40 254 95 31 Fax: +31 (0)40 254 97 79 E-mail : info@atasgl.com Web Site : www.atasgl.com Revision History Document Number: 2406-8030 Date Issue Description 21-10-2011 1.0 Initial issue 15-06-2012 2.0 Sections 4.1.2 and 5.4.1 revised ATAS GL International B.V. Page 2

Contents 1. UNPACKING SYSTEM... 4 2. TOOLS... 4 3. INSTALLATION PREREQUISITES... 4 4. HARDWARE INSTALLATION... 5 4.1 TRAP INSTALLATION... 5 4.1.1 INSTALLATION OF TRAP INTO GC OVEN... 5 4.1.2 GC COLUMN INSTALLATION... 7 4.1.3 ADJUSTING TRAP POSITION... 7 4.1.4 CONNECTING COOLING MEDIA SUPPLY... 7 4.1.5 CRYOTRAP ELECTRICAL CONNECTIONS... 8 5. SOFTWARE INSTALLATION AND CONFIGURATION... 10 5.1 INTRODUCTION... 10 5.2 PC REQUIREMENTS... 10 5.3 INSTALLING EVOLUTION WORKSTATION SOFTWARE... 10 5.4 SETTING UP EXTERNAL COMMUNICATION... 11 5.4.1 USB COMMUNICATION... 11 5.4.2 LAN COMMUNICATION... 13 6. CRYOFOCUS-4 GC RUN/READY SIGNAL CONFIGURATION... 15 7. INSTALLATION VERIFICATION... 16 APPENDIX A: CRYOFOCUS-4 LN2 COOLING LINE CONNECTION DIAGRAM... 17 APPENDIX B: CRYOFOCUS-4 CO2 COOLING LINE CONNECTION DIAGRAM... 18 APPENDIX C: INTERFACE CABLE OPTIC 4 (CRYOFOCUS-4) SHIMADZU GC-2010... 19 ATAS GL International B.V. Page 3

1. Unpacking System Check the contents of the box to the packing lists included with the shipment. The other parts required for the installation are supplied in the CryoFocus-4 - Shimadzu GC-2010 Interface Kit (p/no 2406-4403) and the CryoFocus-4 Cryotrap Kit, LN2 Cooling (p/no 2406-4402, LN2 Cooling) or the CryoFocus-4 Cryotrap Kit, CO2 Cooling (p/no 2406-4408). 2. Tools To perform the installation the following tools are required: 1. 1x cross-tip screwdriver Phillips 1. 2. 1x cross-tip screwdriver Phillips 2. 3. 2x spanner 7/16 inch 4. Hex key 4mm 3. Installation Prerequisites Cooling media/ln2 Cooling: LN2 vessel connection Cooling media/co2 Cooling: CO2 cylinder connection Electrical Power: A pressurized vessel with liquid Nitrogen. Pressure in the vessel should be in the range 100-200 kpa in order for the cooling option to function as specified. ¼ inch Swagelok compatible male pneumatic fitting is required to connect cooling option to the LN2 vessel (not supplied). A high pressure CO2 gas cylinder equipped with a deep (siphon) pipe. 1/8 inch Swagelok compatible male pneumatic fitting is required to connect cooling option to the CO2 cylinder (not supplied). One mains supply outlet is required: AC Single Phase, 100-240V, 50-60 Hz. Warning! The CryoFocus-4 controller must be powered from an earthed (grounded) mains outlet! Controller Location: Interface Cables: The CryoFocus-4 control module is usually placed on the right-hand side of the GC-2010 (when facing the unit). The dimensions of the control module are 35 x 14 x 35 cm (H x W x D). If necessary, the controller can also be placed on the left-hand side of the GC. In case CryoFocus-4 is installed on a stand-alone GC-2010 an Interface Cable OPTIC 4 (CryoFocus-4) - Shimadzu GC-2010 (p/no 2406-4035) is required. ATAS GL International B.V. Page 4

4. Hardware Installation This section describes installation of the CryoFocus-4 trap onto the GC-2010 gas chromatograph. For details of GC-2010 operation refer to the GC-2010 User s Guide. WARNING! An ATAS GL representative must perform instrument installation and configuration. To prevent potential injuries, contact the representative if the instrument must be moved after installation. WARNING! 4.1 Trap Installation It is important that both CryoFocus-4 and host GC are disconnected from the mains supply until the installation is completed. This section should be read carefully in conjunction with CryoFocus- User s Guide. The installation should only be carried out by personnel familiar with the relevant safety regulations and cryogenic operations. The installation of the trap includes 3 steps: 1. Installation of the trap into the gas chromatograph oven; 2. Connections of the trap to a cooling media supply; 3. Electrical connections; 4.1.1 Installation of Trap into GC Oven The trap is mounted vertically or horizontally inside the gas chromatograph oven below the inlet body. A mounting stand (Fig. 4.1) is supplied with the cryotrap. Ideally, the trap should be installed in a location that makes it possible to run the trap hose (cooling line/cables) through the existing holes in the inner and outer panels of the GC oven (e.g. second inlet or detector). If there are no such holes available or free, they will need to be made after choosing their locations carefully. To install the trap, perform the following steps: 1. Determine location for the trap and, if necessary, remove or relocate the second inlet (if fitted). 2. If necessary, make the holes in the oven walls. 3. Install the mounting bracket in a corner of the chromatograph oven close to the inlet to be used with the cryotrap. 4. Carefully guide the trap hose that includes the coolant inlet tube together with the thermocouple and heater cables through the holes in the GC oven wall. 5. Secure the trap to the mounting bracket. Make sure that there is enough space to install the column. ATAS GL International B.V. Page 5

Mounting Stand Trap Trap Mounting Ring Figure 4.1 Trap Mounting Stand ATAS GL International B.V. Page 6

4.1.2 GC Column Installation CAUTION! The cryotrap cannot be used with a metal column. The metal column will shortcircuit the trap heater, causing severe damaged to the trap. A glass capillary pre-column is advised to avoid problems. The column installation depends upon the role that the cryotrap and the GC are to perform. 1. Guide the end of the column through the central tube of the trap. 2. Connect the column to the GC inlet following the instructions for the GC column installation. 3. When installation is completed, all connections should be leak tested with an electronic gas leak detector (e. g. p/no G300025 (LD239)). Under no circumstances should a soap solution or similar be used, as this would contaminate the inlet and the column. 4.1.3 Adjusting Trap Position The trap position should be adjusted to ensure its best performance. Preferably, the central tube of the trap should be aligned with the inlet central axis. CAUTION! When adjusting the position of the trap, special care should be taken not to break the column. 1. Align the trap in all three planes such that its central tube is aligned with the central axis of the inlet. 2. Move the trap up along the mounting rod so that the upper end of the central tube is approximately 5-10 mm from the inlet nut and secure the trap. 3. Inside the column oven, pack mineral wool insulation tightly around the trap hose to ensure that hot air cannot leak out of the oven. 4.1.4 Connecting Cooling Media Supply The CryoFocus-4 trap is cooled directly either by liquid nitrogen or liquid CO 2 supplied from a pressurized LN 2 vessel (not supplied) or a high pressure CO 2 cylinder (not supplied). The high pressure CO 2 cylinder should be equipped with an appropriate siphon tube. In case of LN 2 cooling, in order to achieve fast cooling rate, pressure in the LN 2 vessel should be between 100 to 200 kpa. The CryoFocus-4 trap cooling gas supply diagrams for LN2 and CO2 versions are shown in Appendixes A and B to this guide. Refer to the respective connection diagram while performing the steps described below: ATAS GL International B.V. Page 7

LN2 Cooling Option: 1. Connect one end of the 1/8 inch, 0.5 meter tube (2406-2619) to the trap using 1/8 inch union. 2. Isolate the tube with a piece of the polyethylene foam pipe (2406-2605) of a required length. 3. Connect the OUTLET PORT of the cryogenic valve assembly (2406-4306) to the 1/8 inch tube. 4. Connect one end of the ¼ inch copper tube to a free port of the cryogenic valve assembly via the reducing fitting. Isolate the tube with the remaining part of the polyethylene foam pipe. 5. Decide on the cryogenic valve and the LN2 vessel locations and bend the assembled line accordingly. 6. Connect a free end of just built tube/valve assembly to the LN2 vessel. CO2 Cooling Option: 1. Connect one end of the 1/8 inch, 1.5 meter tube (2406-2606) to the trap using 1/8 inch union. 2. Isolate the tube with a piece of the polyethylene foam pipe (2406-2605) of a required length. 3. Connect the 1/16 to 1/8 inch reducing fitting (2406-2614) to a free end of the 1/8 inch tube. 4. Next, connect one end of the 1/16 inch tube (2406-2608) to the reducing fitting. Isolate the tube with a piece of the polyethylene foam isolation. 5. Connect the OUTLET PORT of the CO 2 cryogenic valve assembly (2406-4307) to a free end of the 1/16 inch tube. 6. Connect a free port of the valve assembly to one end of a short piece of the 1/8 inch tube (2406-2607). Isolate the tube with the remaining part of the polyethylene foam pipe. 7. Decide on the valve and cylinder locations and bend the assembly accordingly. 8. Connect free end of the tube/valve assembly to the CO2 cylinder. 4.1.5 Cryotrap Electrical Connections WARNING! The control unit should be disconnected from the mains supply until all the electrical connections are made. 1. Connect the trap assembly to the CryoFocus-4 control unit using a cryotrap power cable and a thermocouple extension cable supplied with the instrument. ATAS GL International B.V. Page 8

2. Connect C. Valve port on the back of CryoFocus-4 controller to the cryogenic valve. Use the cryogenic valve extension cable supplied with the system. 4.2 Connection to Host GC CryoFocus-4 has a GC interface that permits the system integration with the host chromatograph. The connection is provided on mini-din connector on the rear panel of the control unit. Connect the cable between the GC port of the CryoFocus unit and the Start/Stop terminals on the rear panel of the GC-2010. Use interface cable layout in the Appendix C to this manual to identify the GC connections. 4.3 Connection to Host PC The CryoFocus-4 control unit should be connected to a PC running the CF version of the Evolution Workstation software. USB and LAN communication interfaces are available for this. CryoFocus-4 automatically checks both USB and LAN ports to detect the connection to the host PC. Note that if CryoFocus-4 is connected to a LAN via a switch or a hub, a standard network cable should be used. If the instrument is connected directly to the PC vial the LAN port, a cross-linked network cable is required. For remote communication to be established, the Evolution Workstation software communication parameters should match the communication parameters in the control unit. The details of the communication interface configuration are described in Chapter 5 of this guide. ATAS GL International B.V. Page 9

5. Software Installation and Configuration 5.1 Introduction The Evolution Workstation (CF version) software (also referred to in this guide as control software ) is an integral part of the CryoFocus-4 inlet system. It is designed to perform the following basic functions: Instrument configuration and control Method and sequence definition and development Run time parameters display In addition, Evolution Workstation offers the following features: direct control of the instrument in the standby mode, system run log file. 5.2 PC Requirements Most modern PCs will meet the minimum requirements for the Evolution Workstation software: MS Windows XP, Vista or Windows 7 512 MB of RAM 20 MB free hard disk space USB or Ethernet ports for connection to the CryoFocus-4 control unit 5.3 Installing Evolution Workstation Software To install the Evolution Workstation: Place the CD-ROM in the CD-ROM drive Select the CD-ROM drive in Windows Explorer Double click CryoFocus Evolution Workstation Setup.exe The InstallShield wizard will guide you through the installation process. You can specify the location where the program should be installed. Please note that it should not be installed on a network drive. The program is installed in ATAS program directory on the system C drive. This directory contains two subdirectories for the methods files (file extension MTH) and the sequence files (file extension SEQ). These subdirectories are fixed and cannot be moved to other location. NOTE: If Evolution Workstation is to be uninstalled or updated to a newer version, the subdirectories Methods and Sequences and also their content remain intact after uninstallation. ATAS GL International B.V. Page 10

5.4 Setting Up External Communication After setting up the CryoFocus-4 hardware and installing the PC software, they must first be configured to communicate. Either a USB or a LAN (Ethernet) interface may be used for communication. The CryoFocus-4 controller automatically checks both USB and LAN ports to detect the connection to the host PC. The communication is established if the communication parameters within the controller (USB Serial Port number or IP address) match the external communication parameters set in the Evolution Workstation. In most cases the USB communication should be established first in order to be able to switch to the LAN communication. It is needed to set a valid IP address. 5.4.1 USB Communication Plug the USB cable connected to the CryoFocus-4 controller into an available USB port of the computer. In case a first-time installation, Windows detects a new device and initiates the Found New Hardware Wizard prompting the USB driver installation: 1. When the 'Found New Hardware Wizard' opens, choose option 'No, not at this time' and then click on Next button. 2. Click Install from a list or specific location, then click Next (Fig. 5.1). Figure 5.1 3. When prompted for the device driver location, browse to the Evolution Workstation CD directory USB Serial Drivers. Click Next to continue. Windows should detect the driver as the USB Serial Converter. The driver will be installed. Click Finish to continue. 4. Once the installation of the USB Serial Converter is completed, Windows will prompt you for the installation of a USB Serial Port driver with a new 'Found New Hardware Wizard'. Click the button next to 'No, not at this time' and then Next. Choose again Install from a list or specific location, then click Next. ATAS GL International B.V. Page 11

5. When prompted for the device driver location, browse to the same directory on the Evolution Workstation CD ( USB Serial Drivers ). Click Next to continue. Windows should detect the driver as the USB Serial Port. The driver will be installed. Click Finish to continue. Go to the Device Manager (Control Panel/System/Hardware) to find out the USB serial port number assigned for CryoFocus-4 communication (Fig. 5.2). Alternatively, USB Serial Loopback application can be used to detect the serial port number while connecting OPTIC-4 to the computer after driver installation. The application is supplied on the OPTIC-4 software CD. Note that if port number is greater than 9, it should be manually reassigned to another free port with a lower number. For this, right click on USB Serial Port entry (Fig. 5.2) and select Properties. A new dialog appears. Select Port Settings > Advanced (Fig. 5.2a). In a new dialog change port number assignment to any free port with the number lower than 10. Click OK to confirm. If warning massage appears, click OK to continue. Figure 5.2 Fig. 5.2a ATAS GL International B.V. Page 12

6. Open the Evolution Workstation Software to set the external communication configuration. Select Configuration/ External Communication in the main menu bar and click on the radio button next to USB Serial Port (Fig. 5.3). Select a port number below and click on OK button. The Evolution Workstation should now connect to CryoFocus-4 controller. 5.4.2 LAN Communication Figure 5.3 The default CryoFocus-4 IP address is set to 192.168.0.150. This address can be used for direct CryoFocus-4 to PC LAN communication only. The cross-linked LAN cable should be used in this case. The sub-net mask should be set to 255.255.255.0 and the proxy server settings should be disabled. In order to be able to communicate with CryoFocus-4 via a LAN switch or a hub, the IP address should be changed. The first three segments of a new address should be the same as in the local area network address. The subnet mask should be set to 255.255.255.0. To change the default IP address: 1. Connect the CryoFocus-4 controller to a host PC via USB interface as it is described in the section 5.4.1. 2. Start Evolution Workstation software and select Configuration/ System Configuration. 3. Type a new IP address (Fig. 5.4) and click on OK button. The new address will be sent to the controller. The system configuration dialog will stay open for approx. 35 seconds until controller is automatically rebooted. ATAS GL International B.V. Page 13

Figure 5.4 4. Wait until the CryoFocus-4 is rebooted. Disconnect the USB cable and connect a LAN cable instead. 5. Select Configuration/ External Communication in the Evolution Workstation main menu bar and click on the radio button next to LAN (Fig. 5.3). Click on OK button. The Evolution Workstation should now connect to the device. ATAS GL International B.V. Page 14

6. CryoFocus-4 GC Run/Ready Signal Configuration The CryoFocus-4 Run/Ready signal configuration for GC-2010 installation should be set via Evolution Workstation software as follows: Ready Out Polarity: Run Out Polarity: Closed on Ready Open on Run To set this configuration, go to Configuration/System Configuration menu (Fig. 6.1 ) Fig. 6.1 While within the system configuration dialog, set the options as it is shown in Fig. 6.2 below. Fig. 6.2 Run/Ready Settings ATAS GL International B.V. Page 15

7. Installation Verification This section describes the verification of CryoFocus-4S installation onto Shimadzu GC-2010. Check the neatness of the trap installation. If needed organize the CryoFocus-4 cables and tubing s under GC covers. Set the trap temperature to -150 C (via Standby Configuration) and check if the set point can be reached. It normally takes 2-3 minutes for the first run to reach the set point. Temperature should be stable within ±10 C. Note! Be aware that, in average, the very first run requires a bit more time to cool the trap down compare to the other consequent runs. Create a new CryoFocus method in the Evolution Workstation. Run it to verify the Ready Out signal to GC. The signal is set when the Cryo Low Temperature set point is reached and the CryoFocus is in the Ready state. ATAS GL International B.V. Page 16

Appendix A: CryoFocus-4 LN2 Cooling Line Connection Diagram 2406-2617 ¼ in. Copper Tube, 1.5 m 2406-2618 Reducing Union Inlet 2406-4112 Cryovalve Extension Cable 2406-4038 & 2406-4043 Cryotrap Cables 2406-2605 Thermal Isolation Pipe 2406-4306 LN2 Cryovalve Trap GC Oven CryoFocus-4 LN2 Vessel ATAS GL International B.V. Page 17

Appendix B: CryoFocus-4 CO2 Cooling Line Connection Diagram 2406-2607 1/8 in. Tube, 0.35 m 2406-2608 1/16 in. SS Tube,0.23 m 2406-2614 Reducing Union 2406-2606 1/8 in. SS Tube, 1.5 m 1/8 in. union Inlet 2406-4112 Cryovalve Extension Cable 2406-4038 & 2406-4043 Cryotrap Cables 2406-4307 CO2 Cryovalve 2406-2605 Thermal Isolation Pipe CO2 cylinder with deep pipe 2406-2605 Thermal Isolation Pipe Trap GC Oven CryoFocus-4 ATAS GL International B.V. Page 18

Appendix C: Interface Cable OPTIC 4 (CryoFocus-4) Shimadzu GC-2010 Part number: 2406-4035 1.5 meter, 6 core, Shimadzu GC-2010, loose wires CryoFocus-4, mini-din, male, GC port Wires are numbered as per table below Label: GC2010 Label: OPTIC-4 GC Mini-DIN 6-pin male pin layout Shimadzu GC2010 CryoFocus-4, GC Pin/Wire Signal Type Description Pin Signal Type Description 1 TTL In Start In 1 TTL Out Run Out 2 GND 3 GND 3 TTL Out Ready Out 5 TTL In Ready In 4 GND 6 GND 5 TTL Out Start out 4 TTL In Run in 6 GND 3 GND ATAS GL International B.V. Page 19