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GL Sciences OPTIC-4 User Manual

Multimode gc inlet system
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OPTIC-
Multimode GC Inlet
User's Guide:
Installation and
Operation

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Summary of Contents for GL Sciences OPTIC-4

  • Page 1 OPTIC- Multimode GC Inlet User’s Guide: Installation and Operation...
  • Page 2 Issue 5.3 Disclaimer GL Sciences 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 GL Sciences 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.
  • Page 3 OPTIC-4 User’s Guide Issue 5.3 Revision History Document Number: 2406-8001 Date Issue Description 01-04-2011 Initial issue 18-06-2012 Sections 1.5 and 4.7.3 are changed. Some errors and omissions are corrected. 02-08-2012 Appendix E (Liner Selection Guide) are revised. 15-03-2013 Chapter 4, Appendices E and F are revised.
  • Page 4 Certificate of Conformity to EMC Directive No. 11C00200CRT01 GL Sciences B.V. hereby declares under our sole responsibility that our OPTIC-4 Multimode GC Inlet System when installed in accordance with installation specifications is in conformity with the above Directives and Standards: N.
  • Page 5 GL Sciences does not guarantee that the operation of this product will be uninterrupted or error- free. GL Sciences is not responsible for damage that occurs as a result of your failure to follow the instructions intended for this instrument. The warranty does not apply to consumable parts and...

  • Page 6: Table Of Contents

    ....................... 1.13 冷阱注意事项与警告 ..................... 1.14 1. Mises en garde et précautions d'emploi ................. 1.15 Mises en garde et précautions d'emploi générales concernant OPTIC-4 .... 1.15 1.1.1 Mises en garde générales concernant OPTIC-4 ........... 1.15 1.1.2 Précautions d'emploi générales concernant OPTIC-4 .......... 1.16 Mises et précautions d'emploi concernant le piège cryogénique d' OPTIC ..
  • Page 7 OPTIC-4 User’s Guide Issue 5.3 1.2.1 Avvertenze relative al cryotrap dell’OPTIC-4 ............1.20 1.2.2 Precauzioni relative all’OPTIC-4 cryotrap............. 1.20 2. System Overview ........................2.1 High Performance ....................2.1 Advanced Electronic Flow Control ................. 2.1 Improved Flexibility ....................2.2 Compatibility ......................2.2 3.
  • Page 8 8. Defining and Running Sequences ....................8.1 Defining Sequences using Evolution Workstation Software ........8.1 Running Sequences using Evolution Workstation Software ........8.1 9. Advanced OPTIC-4 Features ...................... 9.1 Automated Solvent Vent Mode ................9.1 Solvent Cooling Effect .................... 9.2 Floating Final Temperature ..................
  • Page 9 Accessories, Consumables, and Spares ..............C.1 Accessories/Upgrades .................... C.2 Installation Kits ....................... C.2 Appendix D: Examples of OPTIC-4 Method Profiles ..............D.1 Split method ......................D.1 Splitless method ....................D.2 Large Volume Injection method ................D.3 LINEX-TD/LINEX-DMI methods ................D.4 Expert method ......................
  • Page 10 OPTIC-4 User’s Guide Issue 5.3 Appendix F: Liner Selection Guide ..................... F.1 Contents Page ix...

  • Page 11: Precautions And Warnings

    1. Use OPTIC-4 for specified types of analyses only. 2. Follow the procedures as written in this manual. 3. Do not modify or disassemble instrument without an express approval of GL Sciences B.V. or its authorized representative as this may compromise safety.

  • Page 12: Operation Precautions And Warnings

    150VA Maximum power consumption: 450 VA 4. Both the OPTIC-4 controller and the host GC must be disconnected from the mains power outlet until installation of the equipment is completed. 5. The Optic-4 controller power switch is located at the rear of the instrument. Leave enough space behind the controller to ensure unrestricted access to the power switch.
  • Page 13 7. Do not tight or lose the top boss or the inlet bottom nut when inlet is at high temperature. The threads can be easily damaged. 8. The OPTIC-4 EFC will be damaged when the inlet pressure exceeds specification. Do not exceed maximum source pressure of 700 kPa.

  • Page 14: Warnings Signs

    OPTIC-4 User’s Guide Issue 5.3 1.4 Warnings Signs HIGH VOLTAGE: Disconnect power cable before removing any units cover. Functional Earth Warning Terminal Label 1.5 Cryogenic Trap Precautions and Warnings The following cautions and warnings relate to the cryotrap fitted to OPTIC-4SC and OPTIC-4DC.
  • Page 15 OPTIC-4 User’s Guide Issue 5.3 extremely cold metal will cause the flesh to stick rapidly and tear when you attempt to withdraw. 5. Cryogenic liquids, when returned to the gaseous state, can displace oxygen from the air under the right conditions. It is strongly recommended to use and store cryogenic liquids in well ventilated areas only.

  • Page 16: Waarschuwingen En Aandachtspunten

    Voor de opslag van oplosmiddelen moet een vlam dovende kast aanwezig zijn en het personeel moet ten alle tijden beschermende kleding en bril dragen. 2. Zowel de GC en de OPTIC-4 moeten afgekoppeld zijn van de netspanning totdat de installatie is afgerond. De OPTIC-4 moet worden aangesloten op een geaarde netspanning.

  • Page 17: Algemene Optic-4 Aandachtspunten

    1.2 Waarschuwingen en aandachtspunten voor de OPTIC-4 Cryotrap De volgende waarschuwingen en aandachtspunten zijn gerelateerd aan de OPTIC-4-SC en OPTIC-4- 1.2.1 Waarschuwingen voor de OPTIC-4 Cryotrap 1. De Cryotrap gebruikt vloeibare stikstof om koud gas te maken voor de lage gebruikstemperaturen.

  • Page 18: Sicherheitshinweise Und Warnungen

    OPTIC-4 User’s Guide Issue 5.3 1. Sicherheitshinweise und Warnungen Dieses Kapitel enthält Erläuterungen zu den bei Installation und Betrieb von OPTIC-4 zu beachtenden Sicherheitshinweisen und Warnungen. Sicherheitshinweise werden an allen relevanten Stellen im Handbuch gegeben. Bitte lesen Sie dieses Handbuch komplett durch, bevor Sie OPTIC-4 installieren oder in Betrieb nehmen. Bei etwaigen Unklarheiten kontaktieren Sie bitte vor der Ingebrauchnahme Ihren Lieferanten.

  • Page 19: Optic-4 - Allgemeine Warnungen

    Instrument schwer beschädigen kann. 1.2 Sicherheitshinweise und Warnungen betreffend die OPTIC-4 Kühlfalle Die folgenden Sicherheitshinweise und Warnungen betreffen die an OPTIC-4-SC und OPTIC-4-DC angebrachte Kühlfalle. 1.2.1 Warnungen betreffend die OPTIC-4 Kühlfalle Die Kühlfalle wird mit flüssigen Stickstoff betrieben um das kalte Gas für Niedrigtemperatur-Betrieb zu erzeugen.

  • Page 20: 注意事项与警告

    本节将说明在安装或操作 OPTIC-4 时应当遵守的警告和注意事项。 安全信息已在手册的相关要点中进行说明。安装或操作仪器前，请完整阅读本手册。如有任何 疑点，请在操作前联系供应商以获取帮助。 备注： 警告、注意事项和其他相关事项的含义约定如下： 警告！ 表示具有潜在危险，若不加以避免，可能导致中度至严重人身伤害或死亡。 小心！ 表示具有潜在危险，若不加以避免，可能导致轻度人身伤害或设备损坏。 强调额外信息，提供此类信息目的是确保合理正确使用此仪器。 注意事项 一般注意事项与警告 4. OPTIC-4 仅用于分析指定的类型。 5. 请按照本手册中描述的流程进行操作。 6. 未经 GL Sciences B.V.或其授权代表批准，请勿改造或拆卸仪器，否则可能会形成安全 隐患。 安装注意事项与警告 OPTIC-4 专为在实验室环境中安装和使用而设计，由经过适当培训的人员操作。安装和调 试仪器前，所有相关的安全事宜均应当按照当地法规进行评估。 8. GL Sciences 代表必须履行仪器安装和配置职责。若仪器安装后必须移动，为防止发生 潜在损坏，应当联系 GL Sciences 代表。 Precautions and Warnings Page 1-10...

  • Page 21: 操作注意事项与警告

    请将仪器安装在通风良好的室内。贮存溶剂时必须采取预防措施，将其存放在防火柜 中，员工必须始终穿着防护服并佩戴护目用具。 10. OPTIC-4 控制器必须使用通地（接地）电源插座供电。 功率要求： 100-240V 交流单相，频率 50-60 Hz。 一般功率消耗： 150VA 最大功率消耗： 450 VA 11. OPTIC-4 控制器和主机 GC 均应当断开供电电源，直到设备安装完成。 12. Optic-4 控制器电源开关位于仪器后面。控制器后面应当留下足够的空间，以方便接触 电源开关。 13. 请勿使用非仪器配用电源线，否则可能导致火灾或触电。 14. 请务必保持进口电力电缆和进口电力终端之间的导电连接良好。连接不良可能导致难 以操作，且可能导致连接件过热。 周围环境： 温度范围： 18 - 40C 湿度： 40 - 70% 8. OPTIC-4 EFC 并非设计使用爆炸性气体（包括氢气）、腐蚀性气体或有毒气体进行操作。...

  • Page 22: 警告标识

    10. 大多数有机溶剂都有一定的毒性。大量溶剂蒸汽可能从排气口排出。我们强烈建议， 使用管道将这些蒸汽输送到排气口配备的通风橱或活性碳阱。但是，不得限制气体从 此排气口排出，以免阻碍仪器的正常运行。 11. 当进行输气管道连接泄露测试时，应当使用适当的电子检漏仪。任何情况下都不能将 肥皂液或类似溶液用作电子检漏仪溶液，否则会污染进口和柱。 12. OPTIC-4 控制装置内存在潜在危险电压。为防止受到人身伤害和仪器损坏，不得拆卸或 改造仪器，亦不得进行内部维修。 13. 操作玻璃内胆时，请务必佩戴必要的防护眼镜，如果内胆因受到冲击而破裂或破碎， 可防止眼睛和皮肤受伤。 14. 操作毛细管柱时，请务必佩戴必要的防护眼镜，如果柱因受到冲击而破裂或破碎，可 防止眼睛受伤。 15. 操作 GC 进口时，进口需要迅速加热至高温。装置关闭或因内部故障而停机后，进口零 件的余温可能保持一段时间。在进口周围作业时，必须小心。更换进口内胆前，请务 必确保进口已冷却（低于 40°C）。 16. 当进口处于高温时，请勿拧紧或拧松顶部凸台或进口底部螺母。螺纹极易受损。 17. 当进口压力超过规定的压力时，OPTIC-4 EFC 可能会损坏。请勿超过最大气源压力 700 kPa。 警告标识 高压： 移除任何装置盖子前，请先断开电力电缆。 Precautions and Warnings Page 1-12...

  • Page 23: 冷阱注意事项与警告

    OPTIC-4 User’s Guide Issue 5.3 警告标记。 功能接地端子。 冷阱注意事项与警告 以下注意事项与警告涉及 OPTIC-4SC 和 OPTIC-4DC 配备的冷阱。 8. 冷阱不得与金属柱共同使用。金属柱会使冷阱加热器短路，造成冷阱严重损坏。建议 使用玻璃毛细管前置柱，以避免出现问题。 9. 冷阱使用低温液体（二氧化碳和液氮）冷却冷阱，使温度低于室温。员工必须完全熟 悉其特性和安全措施才可处理低温液体和冷阱。 10. 低温液体可能造成严重烧伤。处理低温液体时，员工应当始终佩戴防护手套和护目镜 （非安全眼镜）。严禁无保护措施的身体部位接触未绝缘的管子或包含低温产品的零 件。温度极低的金属会迅速粘住皮肤，如果您试图撤离，皮肤会撕裂。 11. 当低温液体恢复气态时，在合适的条件下，可取代空气中的氧气。强烈建议仅在通风 良好的区域使用和贮存低温液体。建议在贮存液氮的区域和通风不良的区域安装氧气 监测仪。 Precautions and Warnings Page 1-13...
  • Page 24 OPTIC-4 User’s Guide Issue 5.3 12. 二氧化碳冷却选项配备一个低温阀，可承受的最大压力达 1000 psi。为避免超过此压力 限制，二氧化碳瓶必须保存在温度低于 25°C 的环境中。 13. 含液氮的杜瓦瓶应当直立处理和贮存。不得使杜瓦瓶倒下或倾斜。 Precautions and Warnings Page 1-14...

  • Page 25: Mises En Garde Et Précautions D'emploi

    1.1 Mises en garde et précautions d'emploi générales concernant OPTIC-4 OPTIC-4 est conçu pour être installé et utilisé en laboratoire par un personnel formé à cet effet. Tous les aspects de la sécurité doivent être déterminés en fonction des règles en vigueur dans les lieux concernés avant d'installer et de mettre en service l'appareil.

  • Page 26: Précautions D'emploi Générales Concernant Optic-4

    Les mises en garde et précautions d'emploi suivantes concernent le piège cryogénique dont sont équipés OPTIC-4-SC et OPTIC-4-DC. 1.2.1 Mises en garde concernant le piège cryogénique d'OPTIC-4 Le piège cryogénique utilise de l'azote liquide pour produire le gaz froid nécessaire aux opérations à...

  • Page 27: Advertencias Y Precauciones

    Hasta que finalice la instalación es imprescindible desconectar de la toma eléctrica tanto el OPTIC-4 como el GC huésped. En cuanto al OPTIC-4 es necesario que reciba la corriente de una toma con conexión a tierra.

  • Page 28: Precauciones Generales Optic-4

    Las advertencias y precauciones siguientes guardan relación con el crioseparador instalado en el OPTIC-4 y el OPTIC-4-DC. 1.2.1 Advertencias relacionadas con el crioseparador del OPTIC-4 El crioseparador utiliza nitrógeno liquido para producir el gas frío necesario para que el instrumento funcione a baja temperatura.

  • Page 29: Avvertenze E Precauzioni

    1.1 Avvertenze e precauzioni generali dell’ OPTIC-4 L’OPTIC-4 é stato progettato per essere istallato e usato in un ambiente di laboratorio da personale adeguatamente preparato. Tutti gli aspetti relativi alla sicurezza devono essere in accordo alle norme locali prima che si proceda all’istallazione e alla commisione dell’apparecchio.

  • Page 30: Precauzioni Generali Dell' Optic-4

    1.2 Avvertenze e precauzioni relative al cryotrap dell’OPTIC-4 Le seguenti avvertenze e precauzioni riguardano il cryotrap inserito all’OPTIC-4-SC e all’OPTIC-4-DC. 1.2.1 Avvertenze relative al cryotrap dell’OPTIC-4 Il cryotrap fa uso di azoto liquido per la produzione di gas freddo per operazioni a basse temperature.

  • Page 31: System Overview

    There is also a ¼ inch version of the inlet, wich works with the ¼ x 3.2 inch thermal desorption tubes. OPTIC-4 can be delivered in one of the five configurations. The basic model is OPTIC-4S. It includes an inlet and a stand-alone electronic controller with the built-in temperature and electronic flow controls (EFC).

  • Page 32: Improved Flexibility

    OPTIC-4 User’s Guide Issue 5.3 other inlet systems, OPTIC-4 has its own GC oven temperature sensor to increase the accuracy of the column flow calculations. Auxiliary EFC unit is a single flow control channel typically used for control of the inlet backflush flow.

  • Page 33: Hardware

    Figure 3.1 OPTIC-4 Controller 3.2 Keypad OPTIC-4 has a simple keypad on the front panel of the unit. Two keys, RUN/END RUN and STANDBY are used for local control of the initialized and running methods. RUN/END RUN key allows to override the standard procedure and run a method while it is being initialized or is in “Waiting for...

  • Page 34: Status Led's

    More extensive control is provided by the Evolution Workstation software running on a host PC. A diagram of the front panel is shown in Figure 3.2. Figure 3.2 OPTIC-4 Control Unit Front Panel 3.3 Status LED’s System status information is presented to the user via the status LED’s: •...

  • Page 35: Rear Panel

    The “Filter” couplings are used to connect the split line filter. The "Aux In" and "Aux Out" couplings on the OPTIC-4-D and OPTIC-4-DC are used for the second (auxiliary) gas channel. This channel can be used, for example, for the inlet backflush flow control.
  • Page 36 GC Oven TC Connection USB and LAN Ports Inlet Cooling Valve Connection Inlet TC and Power Connections Cryotrap Cooling Cryotrap TC and Power Connections Valve Connection Mains Power Inlet Functional Earth Terminal Figure 3.3 OPTIC-4-DC Rear Panel. Hardware Page 3-4...

  • Page 37: Flow Control System

    3.6 Inlet Hardware The OPTIC-4 inlet assembly is installed on the host GC and is connected to the control unit by gas lines and electrical cables. The installation of the inlet on the host GC is described in Chapter 4 “Hardware Installation”, and Figure 3.5 shows the details of the inlet.
  • Page 38 OPTIC-4 User’s Guide Issue 5.3 Side view Cooling Gas in Septum Ferrule Septum Nut Bottom Nut Liner and Inlet Body O-ring Top Boss Top view Gas Lines Cooling Gas In Thermocouple Connector Power Connections Figure 3.5 Inlet Port Hardware Page 3-6...

  • Page 39: Optic-4 Local Control

    • Switch system into the firmware update state. When power is applied to OPTIC-4, a system initialization sequence is performed. During this time all the status LED’s are burning. On completion of the initialization sequence only the LED “STANDBY” remains switched on.

  • Page 40: Pc Control

    3.13 Master/Slave Mode Depending on the way it is connected to the GC and autosampler, OPTIC-4 can be set to act as the system “master” or system “slave” via the configuration menu in the Evolution Workstation software.
  • Page 41 Figure 3.8 OPTIC-4 state diagram in “Slave” mode When the equilibration time is elapsed, OPTIC-4 sets the “Ready Out” (1) signal to the GC. After the injection is completed, OPTIC-4 receives a “Run In” (4) signal from the GC (autosampler) and performs the actions defined in the method.

  • Page 42: Hardware Installation

    4.1.1 Inlet Location If OPTIC-4 is to be used for manual injection only, it can be fitted anywhere on the top of the oven away from the standard GC inlet and detector blocks. The most convenient location is an existing hole in the GC oven's inner skin.

  • Page 43: Inlet Installation

    8. OPTIC-4-SC and OPTIC-4-DC only: the installation and connection of the cryotrap are described in Section 4.6 “OPTIC-4 Cryotrap Installation”. 9. The connection of the OPTIC-4 to the host GC and autosampler is described in Section 1.3 of this chapter and in the manual supplied with the trap installation kit.

  • Page 44: Carrier Gas Line

    The carrier, split, and septum purge lines of the OPTIC-4 inlet are attached to an EFC connection plate. This plate ensures simple and leak free connections of the inlet gas lines to the OPTIC-4 EFC. Remove blanking plate from the “Inlet Gas Lines” port (Fig. 4.1) on the back of the instrument and screw the inlet EFC connection plate instead.

  • Page 45: External Solvent Monitor

    OPTIC-4 User’s Guide Issue 5.3 Septum Purge Line Carrier Line Split Line Figure 4.2 Inlet Gas Lines Connections Designation 4.2.3 Split Line Filter An active carbon filter is installed in the split line in order to protect the EFC from contamination by residual sovent vented through this line.

  • Page 46: Exhaust And Sp Exhaust Ports

    (-180 °) cooling option should be used. For optimum cooling efficiency, standard OPTIC-4 inlet requires a supply of the compressed air at least 500 kPa. A lower pressure supply can be used, but the inlet cooling will work slower. While analytical grade air is not needed, the air supply should be filtered to be free of moisture, oil and particulates.

  • Page 47: Electrical Connections

    3. Connect the inlet thermocouple to the “Inlet TC” connector on the rear panel of the instrument. 4. Install the oven thermocouple supplied with the OPTIC-4 installation kit in the GC oven as close as possible to the oven temperature sensor. Connect the thermocouple to the “GC TC”...

  • Page 48: External Equipment

    OPTIC-4 automatically checks both USB and LAN ports to detect the connection to the host PC. Note that if OPTIC-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 via a LAN port, a crossed network cable is required.
  • Page 49 OPTIC-4 User’s Guide Issue 5.3 Install a column using proper ferrule and the column mounting tool. Push the column through the inlet nut and ferrule (Fig. 4.5). The cone of the ferrule should go into the nut! Avoid the use of the Vespel ferrules as these are likely to cause leaks.

  • Page 50: Cryotrap Installation

    4.7.2 Installation of Cryotrap into GC Oven WARNING! It is essential that both the OPTIC-4 control unit and the host GC are disconnected from the mains supply until the installation is completed. The trap can be mounted either vertically or horizontally inside the gas chromatograph oven. To mount the trap, a mounting stand (see Fig.
  • Page 51 OPTIC-4 User’s Guide Issue 5.3 3. Fix the trap body to the mounting bracket. The spring-loaded screw should be screwed into one of the two holes in the trap body (Fig. 4-6). Use 8 mm spanner to tighten the screw.
  • Page 52 OPTIC-4 User’s Guide Issue 5.3 Figure 4.7 6. Position the trap/mounting stand assembly (Fig. 4.8) within the oven in a way that suits the installation configuration. The trap mounting stand can be positioned either vertically or horizontally. While holding both lower and upper stands, turn the adjustment knob till the stand pads are fixed firmly against the oven side or top/bottom panels.

  • Page 53: Gc Column Installation

    OPTIC-4 User’s Guide Issue 5.3 4.7.3 GC Column Installation CAUTION! The cryotrap cannot be used with a metal column. The metal column will short- circuit the trap heater causing severe damaged to the trap. A glass capillary pre- column is advised to avoid problems.
  • Page 54 OPTIC-4 User’s Guide Issue 5.3 Refer to the respective connection diagram while performing the steps described below: LN2 Cooling Option: 1. Connect the “OUT” port of the cryogenic valve assembly (2406-4306) to the trap. 2. Isolate a part of the trap hose between the GC outer panel and the valve with a piece of the polyolefin foam pipe 12 mm ID (2406-2623) of a required length.

  • Page 55: Cryotrap Electrical Connections

    OPTIC-4 User’s Guide Issue 5.3 4.7.5 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 (2406-4043) supplied with the instrument.

  • Page 56: Software Installation And Configuration

    5. Software Installation and Configuration 5.1 Introduction The Evolution Workstation software (also referred to in this guide as ‘control software’) is an integral part of the OPTIC-4 inlet system. It is designed to perform the following basic functions: • Instrument configuration and control •...

  • Page 57: Communication Parameters

    LAN communication. It is needed to set a valid IP address. 5.4.1 USB Communication Plug the USB cable connected to the OPTIC-4 controller into an available USB port of the computer. In case a first-time installation, Windows detects the new device and will initiate the Found New Hardware Wizard prompting you to install the USB driver: 1.
  • Page 58 Go to the Device Manager (Control Panel/System/Hardware) to find out the USB serial port number assigned for OPTIC-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.

  • Page 59: Lan Communication

    255.255.255.0 and the proxy server settings should be disabled. In order to be able to communicate with OPTIC-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.

  • Page 60: Configuration Parameters

    OPTIC-4 User’s Guide Issue 5.3 Figure 5.4 4. Wait until the OPTIC-4 is rebooted. Disconnect the USB cable and connect a LAN cable to the unit. 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 OPTIC-4 controller.
  • Page 61 “waiting” state is canceled if a Ready or Run input is not received. When the standby timeout is elapsed, OPTIC-4 goes into the standby state. If timeout is set to 0.0 then OPTIC will never go to the standby state but will remain waiting for the signal indefinitely.

  • Page 62: System Configuration Parameters

    OPTIC-4 User’s Guide Issue 5.3 Figure 5.5 5.5.2 System Configuration Parameters Select Configuration/ System Configuration to set the system configuration parameters. Fig. 5.6 shows General tab of the system configuration dialog. Parameters IP Address, Maximum Inlet Temperature, etc. can be set via this dialog.
  • Page 63 OPTIC-4 User’s Guide Issue 5.3 Figure 5.6 Parameters related to the host GC column, carrier gas type, outlet pressure etc. can be set via Column and Carrier Gas Parameters tab (Fig. 5.7) Figure 5.7 Software Installation and Configuration Page 5-8...
  • Page 64 9 Advanced OPTIC-4 Features. Tab GC & AS I/O Configuration (Fig. 5.8) allows to set OPTIC-4 either to Master or Slave mode and chose a correct Ready and Run signals logic level, matching it with the ready and start signals configuration of the host GC and an autosampler (if fitted).

  • Page 65: External Communication

    When this option is enabled, the Modulation Valve group of parameters will appear in every new method opened in the Evolution Workstation control software. The complete list of the system parameters is included in Appendix A “OPTIC-4 Default Parameters”. 5.5.3 External Communication Select Configuration/ External Communication to choose the communication interface to OPTIC-4 (Fig.

  • Page 66: Access Control

    OPTIC-4 User’s Guide Issue 5.3 5.5.4 Access Control Select Configuration/ Access Control to enable the software access control (Fig. 5.10). Figure 5.10 5.5.5 Set Calibration Parameters (Locked) This configuration option is password protected and is intended for the service purposes only.

  • Page 67: Basic Operation

    6. Basic Operation 6.1 Instrument Parameters The OPTIC-4 instrument parameters maintained during the standby state are set from the PC via the Evolution Workstation software. For specific details see section 5.6 of this manual. The run time parameters, including inlet temperature, column flow etc., are set via Evolution Workstation methods.

  • Page 68: Evolution Workstation Status View

    OPTIC-4 User’s Guide Issue 5.3 6.3 Evolution Workstation Status View An example of the Evolution Workstation Status View is shown in Fig. 6.1 below. Title Bar Menu Bar Toolbar Graph View Parameter View Column parameters System Status Error Bar Save Data Status Run Time Display Figure 6.1 Example of EW Status Window...

  • Page 69: Defining And Running Methods

    The OPTIC-4 methods are defined using the Evolution Workstation software running on a host PC connected to the OPTIC-4 control unit. They can either directly initiated from the PC or saved for a later use. Refer, to the Evolution Workstation on-line help for more information about defining and running OPTIC-4 methods.
  • Page 70 7.2.4 LINEX Method OPTIC-4 can be used for an automated thermal desorption analysis of gas and solid samples and also real world samples with complex dirty matrixes. Gas phase samples can be collected off-line using GL Sciences TD liners or adsorption tubes packed with a suitable sorbent.

  • Page 71: Expert Method

    Method Definition To open any of these preprogrammed methods, select File/New menu option. Choose ‘Method’ and click ‘OK’ button. A list of the OPTIC-4 predefined methods will appear on the screen (Fig. 7.1). Figure 7.1 Choose a method which is the most appropriate for your application and click ‘OK’. A method window with the parameter list and the parameters profiles will appear on the on the screen (Fig.
  • Page 72 OPTIC-4 User’s Guide Issue 5.3 See Appendix D “Examples of OPTIC-4 Method Profiles” for all the method types. Figure 7.2 Example of OPTIC-4 LVI Method Set up the method parameters within the method window. Save the method for the later use or send it to OPTIC for immediate execution by selecting Method - Execute.

  • Page 73: Method Parameters

    Evolution Workstation will use a temporary name (e.g. Method1). A method name can be at most 11 characters long. Equilibration Time This parameter is used to ensure the stability of the initial method conditions prior to OPTIC-4 entering the Ready state. End Time This parameter determines the time between the start and end of the GC method run.

  • Page 74: Column Flow Parameters

    OPTIC-4 User’s Guide Issue 5.3 This parameter determines the inlet temperature at the end of the temperature ramp. Hold Time Hold Time is time, during which the inlet temperature is maintained constant. If the Temperature Control is set to ‘Floating’ then the inlet temperature stops being controlled at the end of the thermal segment.

  • Page 75: Solvent Venting Parameters

    OPTIC-4 User’s Guide Issue 5.3 End Column Flow/Inlet Pressure This parameter determines the carrier gas flow (inlet pressure) at the end of the method run. Sample Sweep Column Flow/Inlet Pressure This parameter determines the column flow (inlet pressure) used to sweep the sample with carrier gas prior to desorption (LINEX-TD and LINEX-DMI) or transfer (LVI).

  • Page 76: Auxiliary Outputs

    Flow to reduce the carrier gas use. 7.4.6 Auxiliary Outputs Any of the auxiliary outputs can be used in any of the OPTIC-4 method types. Each output can switch at nine user-specified times during a method run. To keep the Evolution Workstation screens uncluttered, the auxiliary outputs are only shown in the method parameter tables if they have first been selected in Configuration - System configuration - Auxiliary Outputs.
  • Page 77 OPTIC-4 User’s Guide Issue 5.3 Split Flow group: • Initial Split Flow • Split Flow 1 - 9 • Split Flow Time 1 - 9 Auxiliary Flow group: • Start Auxiliary Flow 1 - 9 • Auxiliary Gas Control Time 1 - 9 •...

  • Page 78: Running Methods

    OPTIC-4 User’s Guide Issue 5.3 7.5 Running Methods Figure 7.1 illustrates the states that OPTIC-4 goes through as it runs a method. Startup Standby conditions reached? Standby State Method received? Initialize Method Standby Initial conditions reached ? Ready Standby Run In or...

  • Page 79: Running Method From Evolution Workstation

    Once a method has been saved, you can select Method - Execute menu option to send it to the OPTIC-4 control unit. It will start the method run on OPTIC-4. If you use manual injection, wait for OPTIC-4 to enter the Waiting for Run In state, then inject the sample and select Method – Run menu option or press RUN button on the local interface.
  • Page 80 OPTIC-4 User’s Guide Issue 5.3 Any type of method can be converted to an Expert Method if you want greater control over the method parameters. Select Method/Convert Export Method menu option. Defining and Running Methods Page 7-12...

  • Page 81: Defining And Running Sequences

    OPTIC-4 User’s Guide Issue 5.3 8. Defining and Running Sequences A sequence is a combination of a number of methods. Each method can be run automatically a predefined number of times within a sequence. Sequences can be defined and run using the Evolution Workstation software.

  • Page 82: Advanced Optic-4 Features

    5 to 80 seconds, depending on the solvent type and injection volume and vent flow. The optimization of the vent time is straightforward but can be time-consuming. OPTIC-4 has a solvent monitor (SM) built in the split line of the inlet, which makes it easier to determine the solvent elimination time during the vent transfer.

  • Page 83: Solvent Cooling Effect

    By default, in all OPTIC-4 methods the final inlet temperature is maintained at a constant value until the end of the method. OPTIC-4 has the option of setting the final temperature to ‘floating’ after a specified interval (Hold Time) has elapsed. It is enabled by setting the Temperature Control parameter to ‘Floating’...

  • Page 84: Negative Temperature Ramps In Expert Method

    OPTIC-4 has four auxiliary outputs. These are normally open relays under software control for external devices. Any of the auxiliary outputs can be used in any of the OPTIC-4 methods. To keep the Evolution Workstation screens uncluttered, the auxiliary outputs are only shown in the methods if they have first been selected in Configuration-System Configuration-Auxiliary Outputs.

  • Page 85: Technical Notes

    Temperature Parameters stable Run In,Out End Run Time (min:sec) Figure 9.4 Cryotrap temperature profile. 9.8 Technical Notes For a range of technical notes about the OPTIC-4 inlet and other GL Sciences products, please visit www.glsciences.eu Advanced OPTIC-4 Features Page 9-4...

  • Page 86: Operating Cryogenic Trap

    10.1 Configuring Cryotrap The cryotrap can be used with any of the OPTIC-4 standard method types. Prior to that, it should be enabled in the system configuration. This can be done through the Evolution Workstation software. Ensure that the OPTIC-4 control unit is switched on and communicating with the Evolution Workstation software on the PC.
  • Page 87 OPTIC-4 User’s Guide Issue 5.3 Cryo High Temperature: This is the final temperature, or desorption temperature, to transfer the analytes from the trap to the column. Any temperature between -150 C and +350 C may be set but it is usual to set a temperature in the range +100 C to +350 C.

  • Page 88: Maintenance

    Issue 5.3 Maintenance OPTIC-4 needs little routine maintenance other than replacing consumables. In some cases, the inlet may be affected by contamination and require cleaning. If there are any problems with the operation of the system, please see Chapter 12 “Troubleshooting and Diagnostics”.

  • Page 89: Carrier Gas Leak Check

    11.3 A gas leak in a GC system affects reproducibility and increases consumption of the carrier gas. To check for carrier gas leaks, use an electronic leak detector (GL Sciences p/no 2702-19340 or similar commercial detector). To facilitate the search for a leak, follow the procedure below: 1.
  • Page 90 OPTIC-4 User’s Guide Issue 5.3 8. Wait for a few minutes and verify via the status parameter view in the Evolution Workstation that the standby column flow 20 mL/min is set. 9. Verify that the standby split flow 200 mL/min is set.

  • Page 91: Servicing

    Servicing 11.4 The OPTIC-4 system does not normally require any servicing. If there are problems, which cannot be solved by replacing consumables, cleaning the inlet, or following the troubleshooting instructions, then please contact your supplier for further support.

  • Page 92: Troubleshooting And Diagnostics

    Troubleshooting 12.1 If there is any problem during the installation or operation of OPTIC-4, please check the following issues. 12.1.1 Instrument Does Not Power Up...

  • Page 93: Inlet Cools Down Slowly

    12.2.1 Inlet Thermocouple Fault The error message INJ TC FAULT is generated when the inlet thermocouple fails, or if the TC connection to the OPTIC-4 control unit is lost. This error is displayed in the status pane if the Troubleshooting and Diagnostics...

  • Page 94: Inlet Earth Fault

    The error message INJ EARTH FAULT is generated when the inlet thermocouple loses its connection to the body of the inlet, if the inlet TC connection to the OPTIC-4 control unit is lost or if the earth connection between the inlet base and GC chassis is broken. This error is displayed in the status pane if the problem persists for two seconds or more.

  • Page 95: Cryotrap Temperature Above Maximum

    OPTIC-4 User’s Guide Issue 5.3 pane if the problem exists for two seconds or more. The cryotrap heater controller is shut down. This fault is non-recoverable i.e. the fault must be addressed and the instrument powered off and then on again.

  • Page 96: Auxiliary Flow Warning

    OPTIC-4 User’s Guide Issue 5.3 12.2.13 Auxiliary Flow Warning The AUX FLOW WARNING message is generated when the auxiliary flow set point cannot be reached during the method initialization, method run or standby. This message is displayed in the status pane of the EW on the PC. The software checks that the auxiliary flow is maintained at the set point.

  • Page 97: Technical Specifications

    OPTIC-4 User’s Guide Issue 5.3 Technical Specifications General • Dimensions: 34 cm  14 cm  34 cm (h  w  d) • Weight: 8.4 kg (OPTIC-4DC controller) • Ambient temperature range: 18 - 40C • Ambient operating humidity: 40 - 70% •...
  • Page 98 OPTIC-4 User’s Guide Issue 5.3 External Communication • • • Four auxiliary relay outputs (30V/500 mA max.) • External 24 VDC supply connections (250 mA max.) • Remote start/stop to GC and autosampler Evolution Workstation Software • Method and sequence definition and development •...

  • Page 99: Appendix A: Optic-4 Default Configuration Parameters

    OPTIC-4 User’s Guide Issue 5.3 Appendix A: OPTIC-4 Default Configuration Parameters A.1. Standby Parameters Parameter Name Default Value Allowed Range 35 C -180 - 600 C Inlet Temperature Inlet Temperature Control Yes/No Inlet Cooling ON/OFF Column Flow 1.0 mL/min 0.0 - 20.0 mL/min Split Flow 50.0 mL/min...
  • Page 100 OPTIC-4 User’s Guide Issue 5.3 A.3 GC and Autosampler Input/Output Configuration Parameter Name Default Value Allowed Range OPTIC – Autosampler Ready Out Low to High Low to High /High to Low OPTIC – GC Interface OPTIC Master Master/Slave Ready In...

  • Page 101: Appendix B: Rear Panel I/O Connections

    Ready In TTL In External contact closure or TTL In level change. When contacts Run In are closed or TTL level changed, OPTIC-4 enters Run state Ready Out TTL Out Run Out TTL Out is reversed for 1 sec to generate Run Out signal...

  • Page 102: Auxiliary Outputs

    OPTIC-4 User’s Guide Issue 5.3 Auxiliary Outputs The auxiliary outputs are provided on a sub-D 15 pin female connector. Pin table is shown below. Signal Remarks +24V  20 %. Max. current 250 mA Power output 9(COM), 2(NO), 10(NC) Auxiliary Out 1 Relay output (max.

  • Page 103: Appendix C: Accessories, Consumables, And Spares

    OPTIC-4 Inlet Top Boss Clamp Nut 2406-2013 OPTIC-4 Inlet Clamp Nut Insulator 2406-2015 OPTIC-4 Inlet Septum Nut, Shimadzu type 2406-2016 OPTIC-4 Inlet Septum Nut Insert, Shimadzu type 2406-4020 OPTIC-4 Solvent Monitor Assembly 2406-2250 OPTIC-4 Inlet Cooling Valve 2406-2051 OPTIC-4 EFC Fitting, 1/8" tubing...

  • Page 104: Accessories/Upgrades

    OPTIC-4 Inlet Cooling Kit, Direct LN2 2406-4160 OPTIC-4 Inlet Cooling Kit, CO2 C.6 Installation Kits 2406-4124 OPTIC-4 Installation Kit for Shimadzu 2010 GC 2406-4125 OPTIC-4 Installation Kit for Agilent 7890 GC 2406-4126 OPTIC-4 Installation Kit for Thermo GC Accessories, Consumables and Spares...

  • Page 105: Appendix D: Examples Of Optic-4 Method Profiles

    OPTIC-4 User’s Guide Issue 5.3 Appendix D: Examples of OPTIC-4 Method Profiles Split method Instrument Status Equilibration Time End Time Final Temperature Injector Ramp Rate Temperature Initial Temperature Transfer Column Flow End CF Column Flow Transfer Time Start CF Split Flow...

  • Page 106: Splitless Method

    OPTIC-4 User’s Guide Issue 5.3 Splitless method Instrument Status Equilibration Time End Time Final Temperature Ramp Rate Injector Temperature Initial Temperature Transfer Column Flow End CF Column Flow Transfer Time Start CF Split Flow Split Split Flow Splitless Parameters stable...

  • Page 107: Large Volume Injection Method

    OPTIC-4 User’s Guide Issue 5.3 Large Volume Injection method Instrument Status End Time Final Temperature Equilibration Time Vent Time Ramp Rate Injector Initial Temperature Temperature End CF Column Flow Sample Sweep CF Transfer Time Start CF Vent Flow Split Flow...
  • Page 108 OPTIC-4 User’s Guide Issue 5.3 LINEX method Instrument Status End Time Final Temperature Vent Time Equilibration Time Ramp Rate Injector Initial Temperature Temperature Transfer Time Sample Sweep CF Column Flow End CF Start CF Transfer CF Vent Flow Split Flow...

  • Page 109: Expert Method

    OPTIC-4 User’s Guide Issue 5.3 D.5 Expert method Instrument Status End Time ISO Temp 4 ISO Time 2 ISO Time 4 Equilibration Time Vent Time Ramp Rate 3 ISO Temp 2 ISO Time 1 Ramp Rate 4 Ramp Rate 2...

  • Page 110: Appendix E: Cryogenic Trap Cooling Line Diagrams

    OPTIC-4 User’s Guide Issue 5.3 Appendix E: Cryogenic Trap Cooling Line Diagrams E.1 LN2 Cooling Line Connection Diagram 2406-4112 Cryovalve Extension Cable 2406-2617 2406-2623 ¼ in. Copper Tube, 1.5 m Thermal Isolation Pipe 2406-4038 & 2406-4043 Cryotrap Cables Inlet 2406-2605...
  • Page 111 OPTIC-4 User’s Guide Issue 5.3 E.2 CO2 Cooling Line Connection Diagram 2406-2608 2406-2607 2406-4112 1/8 in. union 1/16 in. SS Tube,0.23 m Cryovalve Extension Cable 1/8 in. Tube, 0.35 m 2406-2614 2406-2606 2406-2623 1/8 in. SS Tube, 1.5 m Reducing Union Thermal Isolation Pipe 2406-4038 &...

  • Page 112: Liner Selection Guide

    Issue 5.3 Appendix F: Liner Selection Guide Notes: 1. All the liners are compatible with the OPTIC-2, OPTIC-3 as well as with the OPTIC-4 standard inlets. 2. Deactivation of liners. The following liners can be deactivated using a high pressures silanization process: 2414-1001, 2414-1005, 2414-1007, and 2414-1013.
  • Page 113 OPTIC-4 User’s Guide Issue 5.3 Liner for Splitless Injections, p/no 2414-1005 This liner is for hot and cold splitless injection of sample volumes below 1 µl. The narrow internal diameter of 1 mm ensures fast transfer of the sample to the column under splitless conditions.
  • Page 114 OPTIC-4 User’s Guide Issue 5.3 Liners for Large Volume Injections These liners have properties that are very well understood. They provide a reliable solution to the majority of the LVI applications. Some liners are packed with proprietary packing materials that were developed for the large volume injections.
  • Page 115 OPTIC-4 User’s Guide Issue 5.3 LINEX-DMI Liners LINEX DMI Liner, p/no 2414-1013 This liner has the small indentations made to hold a sample insert inside. The liner is used for Difficult Matrix Introduction (DMI) in combination with 2406-1010/2406-1020 sample inserts and 2414-1015 needle guide.
  • Page 116 OPTIC-4 User’s Guide Issue 5.3 LINEX-Thermal Desorption Liners Fritted Liner with Single Taper and Frit at 20 mm, p/no 2414-1011 This liner contains a medium porosity frit made from sintered deactivated glass. It can be used for the LINEX direct (in-inlet) thermal desorption of all kind of solid samples. If packed with a suitable packing material, the liner can be used for thermal desorption of gaseous samples.
  • Page 117 OPTIC-4 User’s Guide Issue 5.3 TD Tubes for OPTIC 1/4-inch Version Thermal Desorption Tube, 1/4 x 3.5 inch, p/no 2414-1100 Pack size: 5 pieces. TD Tube 1/4 x 3.5 inch packed with Tenax TA 35/60, 150 mg, p/no 1003-74101 TD Tube 1/4 x 3.5 inch packed with Tenax TA 60/80, 150 mg, p/no 1003-74102 TD Tube 1/4 x 3.5 inch packed with Tenax GR 35/60, 150 mg, p/no 1003-74201...
  • Page 118 OPTIC-4 User’s Guide Issue 5.3 DMI Sample Preparation Block DMI Sample Preparation Block, p/no 2406-2290 The block facilitates the sample preparation handling when using 2406-1010 - OPTIC DMI Sample Insert, 30 L or 2406-1020 - OPTIC DMI Sample Insert, 60 L in combination with 2414-1013 - LINEX DMI Liners.

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