MiDas - Gilson
Transcription
MiDas - Gilson
MiDas™ User’s Guide Gilson, Inc. | PO Box 620027 | Middleton, WI 53562-0027 | Tel: 608-836-1551 OR 800-445-7661 | Fax: 608-831-4451 Gilson S.A.S. | 19, avenue des Entrepreneurs | BP 145, F-95400 Villiers-le-bel, FRANCE www.gilson.com | [email protected] | [email protected] | [email protected] LT319231-01 Table of Contents Safety Electronic and Hazard Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 Safety Notices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 Chemical Hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 Protective Covers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 Stacking Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9 Sécurité Symboles Électroniques et de Dangers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 Notes de Sécurité . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 Risques Chimiques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Précautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Les Capots de Protection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 Sécurité de l’empilement des appareils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 1 Introduction Inspect Shipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 Splitter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 Make Up Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 Direct Sampling Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 Customer Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 Terms and Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 Technical Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 MiDas™ | User’s Guide Table of Contents 2 Installation Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 Plumbing Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 Direct Sampling Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 Splitter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 Make Up Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28 Pressure Bypass Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30 Pressure Relief Valve Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31 Rear Panel Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32 USB Cable Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32 Power Cord Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32 3 Operation Prime the Make Up Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36 Set Make Up Pump Flow Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37 Set Splitter Split Ratio . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37 4 Maintenance Maintenance Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40 Cleaning and Decontamination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40 Direct Sampling Valve Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41 Position Valve for Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41 Remove Valve Driver . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41 Install Replacement Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41 Splitter Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42 Disassemble Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42 Reassemble Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42 Make Up Pump Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Backflush the Pistons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Switch Off the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43 Replace the Pump Head . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44 Clean the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46 Safe State Verification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48 Table of Contents | MiDas™ Troubleshooting Table . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49 Repair and Return Policies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51 Before Calling Us . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51 Warranty Repair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51 Warranty for Non-Gilson Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51 Non-Warranty Repair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51 Return Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 Unit End-of-Life . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 A Replacement Parts B Chemical Compatibility Chart C Appropriate Delivery Rates MiDas™ | User’s Guide Table of Contents 5 Troubleshooting Safety Read this chapter before installing and operating the instrument. Only trained technical personnel in a laboratory environment may use the instrument for non-medical, liquid handling purposes. For safe and correct use of the instrument, operating and service personnel must follow all instructions contained in this guide when installing, cleaning, and maintaining the instrument. All safety precautions must be observed during all phases of operation, service, and repair of the instrument. Failure to comply with these precautions or with warnings described in the user’s guide violates safety standards of design, manufacture, and intended use of the instrument. Gilson assumes no liability for customers failing to comply with these requirements. The instrument has been certified to safety standards required in Canada, Europe, and the United States. Refer to the rear panel label on the instrument and the Declaration of Conformity document for the current standards to which the instrument has been found compliant. MiDas™ | User’s Guide 7 Safety Electronic and Hazard Symbols The following safety symbols and notices may appear on the instrument or in this document: Symbol ~ Explanation Alternating Current Caution Attention Vorsicht WARNING Caution, risk of electric shock Attention, risque de choc électrique Vorsicht, Elektroschockgefahr WARNING Warning, hazardous voltage Avertissement de tensions dangereuses Hochspannung Vorsicht Warning, corrosive chemical Avertissement de substances corrosives Achtung, korrosiven Chemikalien Safety Notices The following safety notices may appear in this document: WARNING WARNING indicates a potentially hazardous situation which, if not avoided, may result in serious injury CAUTION CAUTION indicates a potentially hazardous situation which, if not avoided, may result in minor or moderate injury NOTICE NOTICE indicates a potentially hazardous situation which, if not avoided, may result in equipment damage Chemical Hazards Any chemicals used for analysis should be handled according to good laboratory practice. They should also be stored, used, and disposed of in accordance with the manufacturer’s specifications, as well as local and national regulations. Potentially hazardous chemicals can be used with the MS detector. Use care when handling chemicals and wear appropriate personal protective equipment (PPE). The responsible individual must ensure that personnel are not exposed to hazardous levels of toxic substances as outlined in the Material Safety Data Sheets (MSDS), or any documentation provided by local governing bodies such as The Health Protection Agency (UK) or The Occupational Safety and Health Administration (US). 8 Safety | MiDas™ The following safety precautions concerning the operation of the MS detector and the site in which it is used must be observed at all times in order to prevent injury and damage to the system and associated instruments. Safety Precautions Do not use the instrument if there are signs of visible damage. Do not operate if site conditions are not within specifications. WARNING WARNING Do not override any safety interlock. Do not attempt to operate the instrument with the covers removed. Do not attempt to adjust or replace components other than those that have been described in this user’s guide. The instrument is not designed to be operated in a potentially explosive atmosphere. It is the responsibility of the customer to verify the operating environment meets the requirements of a “non-hazardous area” with regards to potentially explosive atmosphere. WARNING At least two people are required to lift or move the MS detector. Protective Covers Unless specifically instructed, do not remove any protective covers. The product is sealed at the factory. Damage or removal of the warranty seals leads to the loss of liability and warranty entitlements. Stacking Safety Allow sufficient spacing around the MiDas™ for proper cooling and for the connection of mains plug, syringe pump, etc. CAUTION The center of gravity for the MiDas™ is situated towards the front of the unit. Ensure this is observed when positioning or moving the unit. Lifting the unit from the front is recommended. MiDas™ | User’s Guide 9 Sécurité Merci de lire attentivement cette section avant toute installation ou utilisation de l’instrument. Cet instrument est exclusivement destiné à être utilisé dans un environnement de laboratoire, par un personnel qualifié, à des fins de manipulations de liquides non-médicales. Pour une utilisation correcte et en toute sécurité de l’instrument, il est nécessaire que le personnel qui utilise et réalise la maintenance de l’instrument, suive les instructions contenues dans ce guide lors de l’installation, du nettoyage et de la maintenance de l’instrument. Toutes les consignes de sécurité doivent être respectées durant toutes les phases de fonctionnement, d’entretien ou de réparation de l’instrument. Le non-respect de ces précautions ou des avertissements spécifiques mentionnés dans ce guide compromet les normes de sécurité de conception, de fabrication et d’utilisation prévue de l’instrument. Gilson décline toute responsabilité en cas d’incapacité du client à se conformer à ces exigences. L’instrument a été certifié conformément aux normes de sécurité en vigueur au Canada, en Europe et aux Etats-Unis. Merci de vous reporter aux indications mentionnées sur le panneau arrière de l’instrument ainsi qu’au document de Déclaration de Conformité aux normes pour lesquelles l’instrument a été déclaré conforme. MiDas™ | User’s Guide 11 Sécurité Symboles Électroniques et de Dangers Les symboles électroniques et de dangers suivants peuvent apparaitre sur l’instrument: Symbole Signification Alternating current Courant alternatif Wechselstrom ~ Caution Attention Vorsicht Caution, risk of electric shock Attention, risque de choc électrique Vorsicht, Elektroschockgefahr WARNING Warning, hazardous voltage Avertissement de tensions dangereuses Hochspannung Vorsicht Warning, corrosive chemical Avertissement de substances corrosives Achtung, korrosiven Chemikalien Notes de Sécurité Les notes de sécurité suivantes peuvent apparaitre dans ce document: AVERTISSEMENT AVERTISSEMENT: indique une situation potentiellement dangereuse qui, si elle n’est pas évitée, peut entraîner des blessures graves ATTENTION ATTENTION: indique une situation potentiellement dangereuse qui, si elle n’est pas évitée, peut entraîner des blessures mineures à modérées AVIS 12 Sécurité | MiDas™ AVIS: indique une situation potentiellement dangereuse qui, si elle n’est pas évitée, peut entraîner des dégâts matériels Tous les produits chimiques utilisés pour l’analyse doivent être manipulés conformément aux bonnes pratiques de laboratoire. Ils doivent être stockés, utilisés et éliminés conformément aux recommandations du fabricant ainsi qu’à la réglementation locale et nationale. Des produits chimiques potentiellement dangereux peuvent être utilisés avec le détecteur du spectromètre de masse (détecteur MS). Manipuler ces produits avec précaution et porter un équipement de protection individuelle adapté (EPI). Sécurité Risques Chimiques Le responsable doit veiller à ce que le personnel ne soit pas exposé à des niveaux dangereux de substances toxiques comme indiqué dans les fiches de données de sécurité (FDS), ou toute documentation fournie par les instances locales telles que l’Agence de protection de la santé (Royaume-Uni) ou l’Administration de la sécurité et de la Santé (US). Précautions Les consignes de sécurité concernant le fonctionnement du détecteur MS ainsi que l’endroit où il est utilisé, doivent être respectées à tout moment, afin d’éviter tout risque de blessure des utilisateurs, ou tout dommage au système lui-même ou aux instruments associés. Ne pas utiliser le détecteur MS en cas de détérioration visible. Ne pas faire fonctionner si le site présente des conditions non conformes aux spécifications. WARNING AVERTISSEMENT Ne pas désactiver les dispositifs de verrouillage et de sécurité. Ne pas faire fonctionner le détecteur MS sans les capots. Ne pas tenter de régler ou de remplacer des éléments autres que ceux décrits dans le guide de l’utilisateur. Le détecteur MS n’est pas conçu pour une utilisation en atmosphère potentiellement explosive. Il est de la responsabilité du client de vérifier que l’environnement d’exploitation répond aux exigences de ‘’zone non dangereuse’’ en ce qui concerne le risque d’atmosphère potentiellement explosive. AVERTISSEMENT Un minimum de deux personnes est requis pour soulever ou déplacer le détecteur MS. Les Capots de Protection Sauf mention contraire, ne pas retirer les capots de protection. Le produit est scellé à l’usine. Des scellés de garantie endommagés ou absents entraînent l’annulation de la responsabilité et des droits de garantie. MiDas™ | User’s Guide 13 Sécurité Sécurité de l’empilement des appareils Laisser un espace suffisant autour de MiDas™ pour le refroidissement et pour la connexion de prise secteur, pompe seringue, etc. ATTENTION 14 Sécurité | MiDas™ Le centre de gravité du MiDas™ est situé vers l’avant de l’appareil. Prenez en compte lors du positionnement ou pendent le déplacement de l’apparei. Il est recommandée de soulever l’unité par l’avant. 1 Introduction Chapter One This chapter provides information on the following: ●● Inspect Shipment on page 16 ●● Inspect Shipment on page 16 ●● Customer Service on page 17 ●● Terms and Abbreviations on page 17 ●● Trademarks on page 17 ●● Technical Specifications on page 18 MiDas™ | User’s Guide 15 Inspect Shipment Inspect Shipment Upon receipt of the instrument, inspect the exterior of all shipping cartons. All cartons should arrive unopened and undamaged. If examination reveals that damage has occurred in shipment, notify the carrier, and Gilson immediately. Description MiDas™ is an accessory for the VERITY® 1900 MS Detector that includes an integrated make up pump, splitter, and direct sampling valve. The components divert a small portion of flow from the HPLC system to the MS detector, which allow analytes of high concentration to be sampled, allow the reduction of the flow rate to a manageable level and allow flow from the HPLC system to be diluted in an ESI-compatible solvent. Figure 1: MiDas™ Splitter The function of the splitter is to divert a small portion of a flow so that it can be diluted in the make up pump solvent. This allows the MiDas™ to accept samples at saturated concentrations and in non-polar solvents that would be otherwise incompatible with electrospray ionization (ESI). Make Up Pump MiDas™ incorporates a make up pump that dispenses from an external reservoir. This reservoir is filled with an ESI compatible solvent (e.g., water, methanol, acetonitrile, etc.) with the conventional modifiers (such as formic acid, ammonium acetate, etc.). NOTE Care should be taken to ensure that the analyte has moderate solubility in the make up pump solvent so that precipitation does not occur within MiDas™. Direct Sampling Valve MiDas™ features a 2-position, 6-port valve. The recommended operation has a storage loop and syringe port configured as a loop injector. The valve body is polyetheretherketone (PEEK) chosen for its chemical compatibility. NOTE 16 Care should be taken to ensure that the sample does not contain solid particulates that could damage the moving parts. It is recommended to extract the sample through a filter prior to injecting into the valve. Introduction | MiDas™ Gilson, Inc. and its worldwide network of authorized representatives provide customers with the following types of assistance: sales, technical support, applications, and instrument repair. If you need assistance, please contact your local Gilson representative. Specific contact information can be found at www.gilson.com. To help us serve you quickly and efficiently, please refer to Before Calling Us on page 51. Inspect Shipment Customer Service Terms and Abbreviations The following table defines terms and abbreviations that may appear in this document. Term Definition ESI Electrospray Ionization SFI Split Flow Interface m/z ratio Mass-to-charge ratio MSDS Material Safety Data Sheet LED Light Emitting Diode PRV Pressure Relief Valve Trademarks The following trademarks may appear in this document: ●● Microsaic®, Masscape®, and ionchip® are registered trademarks of Microsaic Systems plc in the European Community and the United States. ●● spraychip® is a registered trademark of Microsaic Systems plc in the European Community. ●● vac-chip™ and MiDas™ are trademarks of Microsaic Systems plc in the European Community and the United States. All other trademarks within are trademarks or registered trademarks of Gilson, Inc. MiDas™ | User’s Guide 17 Technical Specifications Technical Specifications MiDas™ Technical Specifications Pump Technical Specification Description Flow Accuracy ±1% at 1 mL/min Flow Range 0.001–9.999 mL/min Max Pressure 400 bar (5802 psi) at 9.999 mL/min Splitter Technical Specification Description Max Pressure 69 bar (1001 psi) Switching Frequency Range 0.2–2.0 Hz Direct Sampling Valve Technical Specification Description Max Pressure 414 bar (6005 psi) Port to Port Volume 0.28–0.50 µL Stop – Stop Actuation Speed 100–280 ms MiDas™ Technical Specifications (continued on page 19) 18 Introduction | MiDas™ Technical Specifications Other Specifications Technical Specification Description Connections USB controlled via VERITY® 1900 MS Detector Dimensions (L x W x H) 36 x 35.5 x 16.5 cm (14.2 x 14 x 6.5 in.) Environmental Conditions Indoor use Altitude: Up to 2000 m Power Requirements Line Voltage: 100–240V AC ±10% Line Frequency: 50/60 Hz Power: 50 W Overvoltage Category II: For transient overvoltages typically present on the mains supply For temporary overvoltage on the mains supply Relative Humidity Operation: 40%–80% Pollution Degree 2: Normally only non-conductive pollution occurs. Occasionally, however, a temporary conductivity caused by condensation must be expected Storage: 10%–90% Temperature Operation: 15°C–30°C Storage : 4°C–40°C Weight 11.8 kg (26 lbs.) MiDas™ | User’s Guide 19 2 Installation Chapter Two This chapter includes information about setup, including: ●● Setup on page 22 ●● Front Panel on page 23 ●● Plumbing Connections on page 25 ●● Rear Panel Connections on page 32 MiDas™ | User’s Guide 21 Setup Setup The diagram shows the main components of the MiDas™. Refer to the labels listed in the table below. The MiDas™ can be stacked on the VERITY® 1900 MS Detector. MiDas™ Components Connection Description M MiDas™ N Front Cover O Gutter P Drain Tube To set up the MiDas™: Figure 2: Exploded View of the MiDas™ 1. Connect the drain tube (P) to the outlet on the gutter. 2. Place the front feet of the MiDas™ through the holes in the gutter. 3. Attach the front cover. Magnets hold it in place and it fits loosely. 22 NOTICE The drip tray (not pictured) is designed to catch minor leaks and should not be relied upon as a permanent part of the fluidics handling. Make sure the fluidics path is constructed out of the correct components and is leak free prior to extended operation. Fix all leaks immediately upon discovery. AVIS Le bac de récupération montré est conçu pour attraper les petites fuites et ne doit pas être perçu comme une partie intégrante de la manipulation fluidique. Assurez-vous que le chemin fluidique construit à partir des composants est correct et sans fuite avant l’utilisation prolongée. Réparez les fuites immédiatement après la découverte. Installation | MiDas™ The figures on the following pages show the ports on the front panel of the MiDas™. Refer to the labels listed below during operation. MiDas™ Front Panel Connection Front Panel Front Panel Description C Direct Access Opening D Communications LED Figure 3: Front Panel with Fluidic Ports Covered E Direct Sampling Valve Refer to Direct Sampling Valve on page 27. F Splitter Refer to Splitter on page 27. G Make Up Pump Outlet Refer to Make Up Pump on page 28. H Make Up Pump Inlet Refer to Make Up Pump on page 28. Figure 4: Front Panel without Cover Showing Fluidic Ports MiDas™ | User’s Guide 23 Front Panel MiDas™ Front Panel Connection Description I Pressure Bypass Assembly Refer to Pressure Bypass Assembly on page 30. J Pressure Relief Valve Assembly Refer to Pressure Relief Valve Assembly on page 31. Figure 5: Location of Pressure Bypass and Pressure Relief Valve Assemblies NOTICE AVIS 24 Installation | MiDas™ Never disconnect the tubing while the unit is in operation. Liquid splashing might cause physical damage. Ne pas débrancher les tuyaux de l’outil durant l’opération. Les éclaboussures peuvent causer d’importants dégâts. Refer to the following diagram when making the plumbing connections described in this chapter. C D D 9A 7B 7C A 1A 2A B A A 3 A 2 4 1 A A 3 7A 6 A 4 Plumbing Connections Plumbing Connections A 5 2B A T 1B 2C E A Z U A D S D 10 F G F 10Plumbing Connections Figure 6: 9B 6 Plumbing Connections Connection Tubing Fitting Input Destination 1A 1/16" OD PEEK Coned 10-32 PEEK Splitter Column Coned 10-32 PEEK Splitter UV/VIS Coned 10-32 PEEK Splitter 4-Way Tee, 0.002" ID Bore 2B Coned 10-32 PEEK Splitter 3-Way Tee, 0.002" ID Bore 2C Coned 10-32 PEEK ¼-28 Flangeless 3-Way Tee, 0.002" ID Bore Backpressure Regulator, 100 psi 1B 2A 1/16" OD 0.005" ID PEEK Plumbing Connections Table (continued on page 26) MiDas™ | User’s Guide 25 Plumbing Connections 26 Plumbing Connections Connection Tubing Fitting Input Destination 3 1/16" OD 0.005" ID PEEK Coned 10-32 PEEK 4-Way Tee, 0.002" ID Bore Make Up Pump Outlet 4 1/16" OD 0.0025" ID PEEK Coned 10-32 PEEK 4-Way Tee, 0.002" ID Bore 3-Way Tee 6 1/8" OD PTFE ¼–28 Flangeless 1/8" Tefzel Make Up Pump Inlet Reservoir 7A 3 mm OD 1 mm ID Silicone Make Up Pump Waste Outlet Waste 7B Make Up Pump Backflushing Inlet Waste 7C Make Up Pump Backflushing Inlet Waste Split Flow Interface Waste 8 1/32" OD 0.010" ID PEEK 9A 1/16" OD 0.020" ID ETFE Coned 10-32 PEEK ¼-28 Flangeless 4-Way Tee, 0.002" ID Bore Backpressure Regulator, 750 psi 9B 1/16" OD 0.020¼ ID ETFE 1/4-28 Flangeless Backpressure Regulator, 750 psi Waste 10 1/32" OD 0.005" ID PEEK ¼-28 Flangeless Coned 6/32 PEEK Backpressure Regulator, 100 psi Inline Microfilter Split Flow Interface Installation | MiDas™ The direct sampling valve has six fluidic ports numbered counterclockwise from 1 as shown in the figure. Refer to the port description in the table below. Direct Sampling Valve Port Specification Ports Description Fluidic Ports Pressure: Tubing: Fitting: 0–60 bar (0–1000 psi) 1/16" PEEK Coned 10-32 PEEK spanner Plumbing Connections Direct Sampling Valve Figure 7: Direct Sampling Valve Diagram Operation Attenuator Flow 2 6 4 5 Inject 1 3 6 4 Syringe 2 1 3 Attenuator Flow Waste Syringe Position 1 5 Load Waste Position 2 Figure 8: Direct Sampling Valve Positions (States) This can be set in two states as shown: 1. Inject: the loop is connected to the splitter and an external pump can deliver the sample for analysis. 2. Load: the loop is connected to the syringe port and waste ready for filling with sample. Splitter The splitter has four fluidics ports as shown. Refer to the port descriptions in the table below and then make the tubing connections. Port Specification for the Splitter Ports Description Fluidic Ports Pressure: Tubing: Fitting: Replacement Part Numbers: Sample side From column Make Up side From make‑up pump To UV/VIS 0–60 bar (0–1000 psi) 1/16" OD PEEK Coned 10-32 PEEK Sample Side 49040130 Make Up Side 490410120 To pressure bypass Figure 9: Splitter Ports Diagram MiDas™ | User’s Guide 27 Plumbing Connections Make Up Pump The make up pump has four fluidics ports as shown below. Refer to the port descriptions in the table below: Backflushing Inlets Make Up Outlet Purge Valve Pump Head Waste Outlet Make Up Inlet Figure 10: Make Up Pump Ports Diagram Make Up Pump Ports 28 Port Description Make Up Pump Outlet Tubing: Fitting: Replacement Part Number: 1/16" ID PEEK Coned 10-32 PEEK 490410120 Waste Outlet Tubing: 3 mm OD 1 mm ID Silicone Backflushing Inlets Pressure : Tubing: 0 bar (0 psi) 3 mm OD 1 mm ID Silicone Make Up Pump Inlet Pressure: Tubing: Fitting: 0 bar (0 psi) 1/8" OD PTFE ¼-28 Flangeless 1/8" Tefzel Installation | MiDas™ NOTE Plumbing Connections Make Up Line to Pump Head Make sure that the tapered side of the ferrule is pointed towards the fitting. 1. Push the tubing (D) through the fitting (C) and ferrule (B). 2. Insert the tubing end as far as possible into the inlet of the pump head (A). 3. Tighten the fitting by hand. Add Solvent to the Make Up Pump Reservoir Bottle WARNING AVERTISSEMENT Potentially hazardous chemicals can be used with the MiDas™. Use care when handling chemicals and wear appropriate PPE. Figure 11: Make Up Line to Pump Head Connection Des produits chimiques potentiellement dangereux peuvent être utilisés avec le MiDas™. Faire preuve de prudence lors de la manipulation des produits chimiques et porter des EPI appropriés. 1. Place the make up reservoir bottle in a suitably ventilated area. 2. Add make up solvent to the make up reservoir bottle. 3. Degas the solvent by sonicating it for ten minutes. 4. Carefully reattach the tubing to the pump and make sure that the filter is immersed in the solvent. 5. It is recommended to prime the make up pump, refer to Prime the Make Up Pump on page 36. MiDas™ | User’s Guide 29 Plumbing Connections Pressure Bypass Assembly Connect a pressure bypass to improve signal stability. This arrangement (shown below) serves to smooth out pressure changes over the splitter cycling. To Splitter Inlet From Splitter Outlet Backpressure Regulator Bypass Outlet To Pressure Relief Valve Assembly Bypass To VERITY® 1900 MS Detector From Make Up Pump Outlet Figure 12: Details of the Fluidic Path in the Pressure Bypass Pressure Bypass Assembly (Part Number 14417010) 30 Component Description From Make Up Pump Outlet Length: Fitting: 1/16" 0.005" ID PEEK x 150 mm 1 x Coned 10-32 PEEK Bypass Tubing: Fitting: 1/16" OD 0.0025" ID PEEK x 90 mm 2 x Coned 10-32 PEEK Splitter Inlet/Outlet Tubing: Fitting: Replacement Part Number: 1/16" OD 0.005" ID PEEK x 60 mm 2 x Coned 10-32 PEEK 490410120 Bypass Outlet Tubing: Fitting: 1/16" OD 0.005" ID PEEK x 60 mm Coned 10-32 PEEK, ¼-28 Flangeless 4-way Tee Fitting: Bore: Coned 10-32 PEEK 0.020" ID 3-way Tee Fitting: Bore: Coned 10-32 PEEK, ¼-28 Flangeless 0.020" ID Backpressure Regulator Fitting: Pressure: ¼-28 Flangeless 7 bar, 100 psi Installation | MiDas™ To protect the splitter from overpressure by the make up pump, a pressure relief valve is present between the pump and the splitter. A pressure in excess of 750 psi (52 bar) causes the relief valve to open and divert flow to waste. The configuration of the pressure relief assembly is shown below. Plumbing Connections Pressure Relief Valve Assembly Figure 13: Flow Path Through Pressure Relief Valve Pressure Relief Valve Assembly (Part Number 14417011) Component Description Relief Valve Inlet Length: 1/16" OD 0.020" ID ETFE x 50 mm Relief Valve (Backpressure Regulator) Fitting: Pressure: ¼-28 Flangeless 52 bar, 750 psi Relief Valve Outlet Tubing: 1/16" OD 0.020" ID ETFE x 1000 mm MiDas™ | User’s Guide 31 Rear Panel Connections Rear Panel Connections Refer to the rear panel diagram and instructions that follow when making rear panel connections. USB communication port Power socket Figure 14: Rear Panel Diagram USB Cable Connection To make the USB cable connection between the MiDas™ and the VERITY® 1900 MS Detector, use the supplied USB cable. Use the end with the “A-type” (flat) connector to connect to the VERITY® 1900 MS Detector and use the end with the “B-type” (square) connector to connect to the MiDas™. Figure 15: USB Cable with “A-Type” Connector Power Cord Connection Locate the appropriate power cord for your line voltage, connect the power cord to the power socket on the MiDas™, and then to a grounded power outlet. The power supply in the MiDas™ accepts any line voltage in the range 100–240 V. There is no voltage selector at the rear of the MiDas™ and there are no externally accessible fuses. Figure 16: USB Cable with “B-Type” Connector After powering up both the VERITY® 1900 MS Detector and the MiDas™, the communications LED should display as solid green. A flashing LED indicates no communication (refer to the Troubleshooting chapter). 32 Installation | MiDas™ WARNING CAUTION WARNING ATTENTION When installing or operating the instrument you must ensure that there is sufficient space behind the instrument to unplug the power cord. Lors de l’utilisation MiDas™ il doit être possible de déconnecter l’appareil de l’alimentation secteur à tout moment. En cas d’urgence, le connecteur d’alimentation de l’instrument doit être facilement accessible et débranchable. Rear Panel Connections When operating MiDas™ it must be possible to disconnect the instrument from mains supply at any time. In the event of an emergency the power connector of the instrument must be easily accessible and removable. Lors de l’installation ou l’utilisation de l’instrument vous devez vous assurer qu’il ya suffisamment d’espace derrière l’appareil pour débrancher le cordon d’alimentation. Never use any cabling not supplied or recommended by Gilson. Use of unspecified cabling may lead to improper operation or failure to comply with safety or EMC regulations. MiDas™ must never be operated from a power outlet that has no ground connection. The absence of a ground connection can lead to electric shock or short circuit. WARNING Never use a power cord other than that supplied by Gilson. The use of an inadequately rated power cord can lead to electric shock or short circuit. WARNING The MiDas™ is used to analyze liquid samples, liquid contact with external equipment may lead to the risk of electric shock or short circuit. The user must ensure that fluidic connections are not close to ancillary equipment and are checked for leaks prior to use. In the event of a leak, any ancillary equipment not designed for use with liquids must be turned off until the liquid is removed. Ne jamais utiliser des câbles non fournis ou recommandés par Gilson. L’utilisation de câbles non spécifié peut entraîner un mauvais fonctionnement ou du non-respect de la sécurité ou de la compatibilité électromagnétique. MiDas™ ne doit jamais être utilisé à partir d’une prise de courant qui n’a pas de connexion à la terre. L’absence de mise à la terre peut provoquer un choc électrique ou un court-circuit. WARNING AVERTISSEMENT N’utilisez jamais un cordon d’alimentation autre que celui fourni par Gilson. L’utilisation d’un cordon d’alimentation non-adéquat peut provoquer un choc électrique ou un court-circuit. MiDas™ est utilisé pour analyser des échantillons liquides, le contact du liquide avec un équipement externe peut entraîner un risque de choc électrique ou de court-circuit. L’utilisateur doit s’assurer que les connexions fluidiques ne sont pas près de l’équipement. MiDas™ | User’s Guide 33 3 Operation Chapter Three This chapter contains information about: ●● Prime the Make Up Pump on page 36 ●● Set Make Up Pump Flow Rate on page 37 ●● Set Splitter Split Ratio on page 37 NOTICE AVIS Condensation caused by relocating MiDas™ to new ambient conditions could cause hardware failure within MiDas™. Allow device to acclimatise for three hours before powering on a recently moved system. La condensation provoquée par le déplacement du MiDas™ dans de nouvelles conditions ambiantes pourrait provoquer une défaillance. Laissez MiDas™ s’acclimater pendant three heures avant de mettre l’appareil sous tension. MiDas™ | User’s Guide 35 Prime the Make Up Pump Prime the Make Up Pump NOTICE Running the pump when dry can cause damage to the pump. Ensure that the pump has been primed and pistons have been backflushed (refer to Backflush the Pistons on page 43) before starting pumping. Check regularly that the make up pump solvent reservoir contains enough fluid and does not run dry during operation. Utiliser la pompe à l’état sec peut causer des dommages à la pompe. Assurezvous que la pompe a été amorcée et les pistons ont été contre-rincés (Backflush the Pistons on page 43) avant de commencer le pompage. AVIS Vérifiez régulièrement que le réservoir de maquillage contient suffisamment de liquide et ne tarit pas en cours de fonctionnement. Back Flushing Inlets Refer to the diagram when following this procedure. 1. Make sure that the filter is immersed in the make up reservoir. Make Up Outlet 2. Twist the black purge valve one turn counterclockwise to open it. 3. Attach the supplied plastic syringe using the metal adaptor and silicone tubing to the waste outlet. Purge Valve Pump Head 4. Draw 5–10 mL of solvent from the reservoir by repeatedly filling the syringe, detaching Waste Outlet it, and then emptying to an appropriate waste container. 5. Connect one end of the silicone tubing to the metal pipe of the purge valve and the other to a solvent waste container. Make Up Inlet Figure 17: Make Up Pump Ports Diagram 6. Prime the pump for a few minutes at high flow (5–10 mL/min). 7. When satisfied that the line to the pump is filled and liquid is being drawn through the pump in a continuous stream, stop the pump and then shut the purge valve by turning it fingertight clockwise. The pump is now primed and ready to dispense make up pump solvent. NOTE 36 This operation should be performed on any change to the make up composition to avoid the possible appearance of solvent fronts mid-experiment. Inappropriately fast flow rates can lead to sample outgassing and bubble formation. These bubbles may alter dispensed volume and hence sample accuracy. Operation | MiDas™ Set the make up pump flow rate at an appropriate level so that after splitting in the split flow interface (SFI), the spraychip receives no more than 2 µL/min. The standard split ratio supplied with the VERITY® 1900 MS Detector is 1000:1. With the supplied spilt the maximum should therefore be 2000 µL/min (2 mL/min). If greater dilution is required then the VERITY® 1900 MS Detector split can be adjusted to a higher ratio (refer to the VERITY® 1900 MS Detector User’s Guide for details on adjusting the split). NOTE Use of higher source flow rates than 2 µL/min can lead to unreliable electrospray ionization (ESI) conditions and shortened spraychip® and vac-chip™ lifetimes. Set Splitter Split Ratio Set Make Up Pump Flow Rate Set Make Up Pump Flow Rate The split ratio of the splitter should be set to a level appropriate for the application, and can be set by program number or by allowing the software to calculate the split factor. Care should be taken to ensure resultant flow rates are compatible with the VERITY® 1900 MS Detector (refer to the VERITY® 1900 MS Detector User’s Guide). H PLC Flow Rate (mL/min) Split Ratio Figure 18: Recommended Split Factor Based on Flow Rate and How to Calculate a Split Ratio Source: Data from MRA™ Operating Manual, Rheodyne, L.P., 2320949A(1), 8/01. MiDas™ | User’s Guide 37 4 Maintenance Chapter Four The following maintenance may be carried out by users: ●● Direct Sampling Valve Replacement on page 41 ●● Splitter Service on page 42 ●● Replace the Pump Head on page 44 ●● Clean the Check Valves on page 46 You are only permitted to perform the maintenance tasks described in this user’s guide. If additional maintenance is required, contact your local Gilson representative (refer to Customer Service on page 17). MiDas™ | User’s Guide 39 Maintenance Preparation Maintenance Preparation Before maintenance can begin, the MiDas™ must be decontaminated by removing any hazardous chemicals used by the instrument. Further, the instrument should be disconnected from any other instrument and the unit MUST be disconnected from the power supply. To protect the electronic components of the MiDas™ from ESD, the rear chassis of the MiDas™ should be connected to an electronic ground either through the ground pin in the mains power supply or a grounding clip. After disconnecting the unit from the mains, wait at least one minute before attempting any maintenance. WARNING CAUTION WARNING ATTENTION When operating MiDas™ it must be possible to disconnect the instrument from mains supply at any time. In the event of an emergency, the power connector of the instrument must be easily accessible and removable. Lors de l’utilisation MiDas™ il doit être possible de déconnecter l’appareil de l’alimentation secteur à tout moment. En cas d’urgence, le connecteur d’alimentation de l’instrument doit être facilement accessible et débranchable. Cleaning and Decontamination Even if contamination is not suspected or seen, the exterior surfaces of the MiDas™ should be wiped down with 10% aqueous IPA to remove any residues. If any parts of the assemblies need to be removed or disassembled then these parts should also be checked for signs of contamination. The fluid lines should be flushed with 10% aqueous IPA to remove any residues inside the system. Potentially hazardous chemicals can be used with the MiDas™. Use care when handling chemicals and wear appropriate PPE. WARNING AVERTISSEMENT 40 Maintenance | MiDas™ Des produits chimiques potentiellement dangereux peuvent être utilisés avec le MiDas™. Faire preuve de prudence lors de la manipulation des produits chimiques et porter des EPI appropriés. Position Valve for Replacement Ensure that the valve driver is in the correct orientation for replacement of the valve (position 1). Remove Valve Driver After positioning the valve as described above, remove all fluidics connectors and loosen the spanner that holds the valve in place. Remove spanner completely. Do not use a wrench for this step. Spanner should be tightened and loosened using only your hand. Direct Sampling Valve Replacement Direct Sampling Valve Replacement Figure 19: Correct Orientation of the Direct Sampling Valve with Ports 1, 2, and the Clocking Groove at the Top Install Replacement Valve The shaft of the replacement valve must be oriented in Position 1 prior to insertion into the valve driver body. In Position 1, the flat of the shaft is oriented perpendicular to the marking on the reverse of the valve body. Insert the valve into the valve driver in the orientation shown in the figure above and note the orientation of the numbered ports. Ports 1, 2, and narrow clocking groove will always be at the top when the valve driver body is oriented correctly. MiDas™ | User’s Guide 41 Splitter Service Splitter Service Normal use of the splitter will provide one million samplings. The main cause of early failure, which is seen as valve leakage, is abrasive particles in the sample and/or mobile phase or precipitation of concentrated solutions. Either can cause scratches on the rotor seal and stator face assembly. In order to service the splitter, you will need to obtain a splitter maintenance kit (part number 18007044). Disassemble Valve To disassemble the splitter valve, refer to the figure above, and then proceed as follows: 1. With the hex key provided in the splitter maintenance kit, remove the stator screws from the stator. 2. Remove the stator and stator face assembly from the stator ring. The stator face assembly usually remains on the stator. 3. Remove the stator ring. 4. Remove the rotor seal from the valve body. The rotor seal is mounted on three pins and can be pulled off. Reassemble Valve NOTE Before reassembly, use clean, filtered compressed gas to blow out the shaft assembly area of the valve. 1. Mount the new rotor seal with the slots facing the stator. The three pins on the shaft assembly fit into the mating holes in the rotor seal only one way. Figure 20: Exploded View of the Splitter 2. Replace the stator ring so the two short pins enter the mating holes in the body. 3. Mount the new stator face assembly onto the stator. The pins on the assembly fit into the mating holes on the stator only one way. 4. Replace the stator and stator face assembly on the valve so that the pin in the stator ring enters the mating hole in the stator. 5. Replace the stator screws into the stator. Tighten each an equal amount until the screws are fingertight, then turn another half turn. 42 Maintenance | MiDas™ Make Up Pump Service Make Up Pump Service Backflush the Pistons When you flush the pistons regularly, the service life of the seals and pistons increases. While flushing, contaminants are washed from the rear piston area. Refer to the figure below when attempting this operation. Flushing Solution The following solvents are recommended for flushing the pistons: Figure 21: Flushing the Pistons in the Pump Head ●● Water ●● Mixture of 80% water and 20% ethanol ●● Isopropanol 1. Open the black purge valve adjacent to the pump head. 2. Connect the outlet to the waste container with a length of supplied silicone tubing (1). 3. Connect the inlet to the syringe filled with flushing solution with the supplied silicone tubing (2). 4. Fill up flushing solution with the syringe through the pump head until there are no more air bubbles running through the waste bottle. 5. Afterwards, remove the tubing 1 and tubing 2 and connect inlet and outlet with a tubing. Switch Off the Pump If you want to switch off the pump for a longer term, flush the pump head with isopropanol. MiDas™ | User’s Guide 43 Make Up Pump Service Replace the Pump Head Aggressive or toxic solvent residue can irritate the skin! Wear appropriate PPE. WARNING Les résidus de solvant agressif ou toxique peuvent irriter la peau! Porter des EPI appropriés AVERTISSEMENT NOTICE AVIS Mishandled piston rods can break. Before disassembling the pump head, remove the two piston rods and deposit in the correct orientation. When assembling the pump head, the piston rods must be inserted on the same side they have been removed from. Les tiges de piston maltraitées peuvent se briser. Avant de démonter la tête de pompe, enlever les deux tiges de piston et posez-les dans le bon sens. Lors du montage de la tête de pompe, les tiges de piston doivent être insérés sur le même côté dont ils ont été retirés. Remove the Pump Head NOTE Ensure that the pump head has been flushed with suitable solvent. 1. Unscrew inlet fitting (2) and outlet fitting (1). 2. Unscrew the inlet fitting (5). 3. Unscrew the outlet fitting (4) to the pressure sensor. 4. Alternately unscrew the four fastening screws (3). 5. Hold the pump head and consecutively pull out all fastening screws. Figure 22: Pump Head 44 Maintenance | MiDas™ 1. Insert the fastening screws (3) and tighten alternately. 2. Tighten the outlet fitting (4) to the pressure sensor. 3. Tighten the inlet fitting (5). 4. Tighten the inlet fitting (2) and the outlet fitting (1) of the piston. NOTICE AVIS Overtightening capillary fittings can damage the pump head. Check the torque of screw fittings. Appropriate torques is 5 Nm for stainless steel fittings and 0.5 Nm for PEEK fittings. Make Up Pump Service Install the Pump Head Le serrage des raccords capillaires peut endommager la tête de la pompe. Vérifiez le couple des raccords vissés. Les couples appropriés sont de 5 Nm pour des raccords en acier inoxydable et 0,5 Nm pour les raccords en PEEK. MiDas™ | User’s Guide 45 Make Up Pump Service Clean the Check Valves Dirty check valves do not open and close properly. They can cause pressure fluctuations and irregular flow. Figure 23: Pump Head NOTE Ensure that the pump head has been flushed with suitable solvent. Remove the Check Valves NOTE Loosen the screw fittings of the capillary connections alternately, to prevent the capillaries from bending. Pump head should be flushed prior to procedure. 1. Unscrew the inlet fitting (1) and the outlet fitting (2). Remove the check valve. 2. Unscrew the inlet fitting (5) and remove the check valve. Clean the Check Valves 1. Fill a beaker with solvent. 2. Place the valve in the beaker. 3. Put the beaker in an ultrasonic bath for at least ten minutes. 46 Maintenance | MiDas™ NOTE Make Up Pump Service Install the Check Valves Insert the valves in the direction of flow as shown in the figure below. Figure 24: Check Valve Showing Ball (1) and Flow Direction (2) 1. Insert the check valve and tighten the inlet fitting (5). 2. Insert the check valve. Tighten the inlet fitting (1) and the outlet fitting (2). 3. Tighten the outlet fitting (2) and the inlet fitting (5) with 7.5 Nm. MiDas™ | User’s Guide 47 Safe State Verification Safe State Verification After maintenance, the MiDas™ should be tested to verify that it is in a safe state. Monitor the make up pump pressure at 1000 µL/min (1 mL/min) when infusing methanol, 0.1% formic acid through the split flow interface (SFI). If the pressure is not within 10–25 bar, then immediately switch off the MiDas™ and disconnect the instrument from the mains power supply and any attached equipment. Do not use the instrument. Contact Gilson. WARNING CAUTION WARNING ATTENTION When operating MiDas™ it must be possible to disconnect the instrument from mains supply at any time. In the event of an emergency the power connector of the instrument must be easily accessible and removable. Lors de l’utilisation MiDas™ il doit être possible de déconnecter l’appareil de l’alimentation secteur à tout moment. En cas d’urgence, le connecteur d’alimentation de l’instrument doit être facilement accessible et débranchable. Potentially hazardous chemicals can be used with the MiDas™. Use care when handling chemicals and wear appropriate PPE. WARNING AVERTISSEMENT 48 Maintenance | MiDas™ Des produits chimiques potentiellement dangereux peuvent être utilisés avec le MiDas™. Faire preuve de prudence lors de la manipulation des produits chimiques et porter des EPI appropriés. 5 Troubleshooting Chapter Five Make sure the VERITY® 1900 MS Detector is fully operational first. Refer to the VERITY® 1900 MS Detector User’s Guide troubleshooting chapter for details. Troubleshooting Table Symptom Cause Remedy MiDas™ does not respond to commands. No communications (communication LED on MiDas™’ front panel flashes constantly). Check the USB connection between the MiDas™ and the VERITY® 1900 MS Detector. Check that the USB smartlock software dongle has been connected and then reboot the software. MiDas™ is not powered up (communication LED on MiDas™ front panel is off ). Check power connection. I have no signal during sampling acquisition. The VERITY® 1900 MS Detector is not ready for a sampling experiment. Refer to the VERITY® 1900 MS Detector User’s Guide for troubleshooting advice. I have signal, but cannot see my direct sample. Excessive chemical noise is swamping signal. Refer to the VERITY® 1900 MS Detector User’s Guide for troubleshooting advice. The splitter is not operating (MiDas™ is generating a constant ‘pulsing’ sound) Contact Gilson. The loop injection is not operating (MiDas™ should emit an audible ‘click’ when switching the valve). Contact Gilson. MiDas™ | User’s Guide 49 Symptom Cause Remedy Make up pump solvent is not dispensed or flow rate/pressure is erratic. Pump not primed. See Prime the Make Up Pump on page 36. Inlet solvent flow blocked. Check reservoir level. Check reservoir filter and replace, if necessary. Check valves blocked. See Clean the Check Valves on page 46. Check valves defective. See Clean the Check Valves on page 46. Pump head seals defective. If liquid emerges behind the pump head in the back flush, contact Gilson. The pressure rating of the valve has been exceeded. Check that the flow path is not blocked causing abnormal back pressure, and then reduce flow rates to the splitter to reduce pressure. The rotor seal and stator face assembly have been damaged by abrasive particles in the sample and/or mobile phase or crystallization of buffer solutions. Replace the stator/rotor and contact Gilson for a maintenance kit. Note: Flush the valve frequently to prevent crystallization. Splitter leaks between the stator and stator ring. 50 Troubleshooting | MiDas™ Before Calling Us Your local Gilson representative will be able to serve you more efficiently if you have the following information: ●● Serial number and model number of the instruments involved ○○ The serial number is located on the rear panel ●● Installation procedure you used ●● List of concise symptoms Repair and Return Policies Repair and Return Policies ●● List of operating procedures and conditions you were using when the problem arose ●● List of other devices connected to the instrument and a description of those connections ●● List of other electrical connections in the room ●● Diagnostics report Warranty Repair Units covered under warranty will be repaired and returned to you at no charge. If you have any questions about applicability, please contact your local Gilson representative. Warranty for Non-Gilson Equipment Contact your local Gilson representative. Gilson, Inc. will coordinate with the manufacturer for handling warranty-related service. The warranties are those provided by the manufacturer. Non-Warranty Repair For out-of-warranty repairs, contact your local Gilson representative who will discuss service options with you and can assist in making arrangements to return the equipment, if necessary. MiDas™ | User’s Guide 51 Repair and Return Policies Return Procedure Contact your local Gilson representative to obtain authorization before returning any Gilson equipment. To return a piece of equipment: ●● Carefully pack the unit to prevent damage in transit. Check with your local Gilson representative regarding proper method of shipment. No responsibility is assumed by Gilson or your local Gilson representative for damage caused by improperly packaged instruments. Indicate the authorization on the carton and on the packing slip. ●● Always insure for the replacement value of the unit. ●● Include a description of symptoms, your name, address, phone number, and purchase order to cover repair costs, return and shipping charges, if your institution requires it. Unit End-of-Life When a unit reaches the end of its useful life, refer to www.gilson.com for directions and information on the end-of-life policy. This is in accordance with the European Union Directive 2002/96/EC on Waste Electrical and Electronic Equipment (WEEE). 52 Troubleshooting | MiDas™ A Replacement Parts Appendix A Part Number Description 14417010 VERITY 1900, MIDAS PRESSURE BYPASS ASSY 14417011 VERITY 1900, MIDAS PRES RELIEF ASSY 14417012 VERITY 1900, MIDAS INJ VLV REBUILD KIT 14417013 VERITY 1900, MIDAS PUMP CHECK VLV 18007044 MRA SPLITTER MAINTENANCE KIT 490410120 F120, FINGERTIGHT FITTING Used for Make Up Pump Outlet and Splitter Make Up Side 49040130 NUT,LONG FINGER TIGHT,PEEK NAT, (F-130) Used for Splitter Sample Side MiDas™ | User’s Guide 53 B Chemical Compatibility Chart Appendix B This appendix allows you to either check which materials will work with the chemicals you are using or planning to use; or to view what compatibility rating given to a material you are planning to use. Provided courtesy of IDEX Health & Science LLC Chemical rating key: A = Minor Issue. NOTE The substance has little interaction with the material. Prolonged exposure may cause material deterioration. B = Use Caution. NOTE The substance has slight interaction with the material. Be cautious when using with tubing and frits. Exposure may cause material deterioration C = Incompatible. NOTE The substance is not recommended to be used with the material. Chemical Compatibility Chart Substance Fraction Acetic anhydride Aluminum acetate 100% Aluminum chloride Severity Material Notes B Stainless Steel B Stainless Steel C Stainless Steel Aluminum hydroxide 10% B Stainless Steel Aluminum sulfate 100% B Stainless Steel Ammonium bicarbonate 90% B Stainless Steel Chemical Compatibility Chart (continued on page 56) MiDas™ | User’s Guide 55 Chemical Compatibility Chart Chemical Compatibility Chart Substance Fraction Ammonium carbonate Severity Material Notes B Stainless Steel Elevated temperatures may reduce resistance. Elevated temperatures may reduce resistance. Ammonium chloride 10% B Stainless Steel Ammonium oxalate 10% B Stainless Steel Ammonium sulfite 10% B Stainless Steel Aniline 10% B Stainless Steel Anisole B UHMWPE Aqua regia C PEEK, UHMWPE Barium carbonate B Stainless Steel B Stainless Steel Barium nitrate B Stainless Steel Barium sulfate B Stainless Steel Benzene B Stainless Steel, UHMWPE Benzene sulfonic acid C PEEK B Stainless Steel B UHMWPE B Stainless Steel C PEEK C PEEK, UHMWPE Bromine water C Stainless Steel Bromochloromethane C UHMWPE Barium chloride Benzoic acid 10% 60% Benzoyl chloride Boric acid 100% Bromine (dry) Bromine (wet) saturated Elevated temperatures may reduce resistance. Butyric acid 100% B Stainless Steel Calcium carbonate 100% B Stainless Steel Calcium chlorate 10% B Stainless Steel Calcium chloride 10% C Stainless Steel Chemical Compatibility Chart (continued on page 57) 56 Chemical Compatibility Chart | MiDas™ Substance Fraction Calcium hydroxide 50% Severity Material Notes B Stainless Steel B Stainless Steel B Stainless Steel Carbon disulfide B Stainless Steel, UHMWPE Carbon tetrachloride B Stainless Steel, UHMWPE Carbonic acid B Stainless Steel Chloric acid C Stainless Steel B Stainless Steel Chlorine C PEEK ,UHMWPE Chlorine gas B Stainless Steel, UHMWPE Chlorine liquid B PCTFE, UHMWPE Elevated temperatures may reduce resistance. Chlorobenzene B PCTFE Elevated temperatures reduce resistance. Chloroform B PCTFE A PEEK Not recommended for use with PEEK rotor seals. B UHMWPE C PEEK, UHMWPE B PCTFE B Stainless Steel C PEEK Calcium sulfate Carbolic acid Chlorinated water Chlorosulfonic acid 100% saturated 10% Chlorotrifluoroethylene Chromic acid conc. Citric acid 10% B Stainless Steel Copper carbonate 10% B Stainless Steel Copper chloride 5% aerated C Stainless Steel Subject to pitting. Elevated temperatures and prolonged exposure may reduce resistance. Chemical Compatibility Chart Chemical Compatibility Chart Subject to pitting. Subject to pitting. Chemical Compatibility Chart (continued on page 58) MiDas™ | User’s Guide 57 Chemical Compatibility Chart Chemical Compatibility Chart Substance Fraction Severity Material Notes Copper cyanide 100% B Stainless Steel Copper sulfate 100% B Stainless Steel Creosote oil B Stainless Steel Cyanogen gas B Stainless Steel Dichlorobenzene (o-) B UHMWPE Elevated temperatures may reduce resistance. Dichlorobenzene (p-) B UHMWPE Elevated temperatures may reduce resistance. Dichloroethylene C UHMWPE Dimethylsulfoxide (DMSO) B PEEK Be cautious when using with tubing and frits. Diphenylsulfone (DPS) B PEEK Be cautious when using with tubing and frits; elevated temperatures reduce resistance. Dowtherm A C PEEK Dowtherm G B PEEK Dowtherm HT B PEEK Dowtherm LF B PEEK Ethyl acetate B Stainless Steel Ethyl ether B PCTFE Ethyl glycol B Stainless Steel Ethylene bromide B PCTFE Ethylene chloride (dichloroethane) B UHMWPE Ethylene oxide C PCTFE Ferric chloride B PEEK C Stainless Steel Elevated temperatures reduce resistance. Elevated temperatures reduce resistance. Chemical Compatibility Chart (continued on page 59) 58 Chemical Compatibility Chart | MiDas™ Chemical Compatibility Chart Chemical Compatibility Chart Substance Fraction Severity Material Notes Ferric nitrate 10% B Stainless Steel Ferric sulfate 100% B Stainless Steel Ferrous chloride C Stainless Steel Ferrous sulfate B Stainless Steel Fluorine C PEEK, UHMWPE Formic acid B Stainless Steel, PEEK Freon 11 B PCTFE Furfural B Stainless Steel Room temperature only. Gallic acid 100% B Stainless Steel Glycerin 100% B Stainless Steel B UHMWPE Halothane Hydrobromic acid 10% conc. C Elevated temperatures may reduce resistance. PEEK Hydrochloric acid C Stainless Steel Hydrocyanic acid B Stainless Steel Hydrofluoric acid (40%) C PEEK Hydrofluosilic acid C Stainless Steel Hydrogen peroxide 100% B Stainless Steel Hydrogen sulfide 100% B Stainless Steel B PEEK C Stainless Steel Iodine Room temperature only. Lactic acid 100% B Stainless Steel Magnesium chloride 50% B Stainless Steel Magnesium sulfate 100% B Stainless Steel B Stainless Steel Malic acid Chemical Compatibility Chart (continued on page 60) MiDas™ | User’s Guide 59 Chemical Compatibility Chart Chemical Compatibility Chart Substance Fraction Mercuric chloride 10% Severity Material Notes B PCTFE C Stainless Steel Mercury 100% B Stainless Steel Methyl alcohol 100% B Stainless Steel Methylcyclohexane B UHMWPE Elevated temperatures may reduce resistance. Methylene chloride A PEEK B UHMWPE Be cautious when using with tubing and frits; Room temperature only. Not recommended for use with PEEK rotor seals. C Stainless Steel Muriatic acid Naptha 100% B Stainless Steel Nickel chloride 100% B Stainless Steel Nitric acid 30% conc. B PEEK, Stainless Steel, UHMWPE Prolonged exposure may cause deterioration. Nitrogen tetroxide B PCTFE Below Room Temperature Oils (linseed and olive) B UHMWPE Oleic acid B Stainless Steel Oleum C PEEK, UHMWPE Oxalic acid 10% B Stainless Steel Elevated temperatures may reduce resistance. Ozone liquid B UHMWPE Elevated temperatures may reduce resistance. Phenol 100% B Stainless Steel C PEEK Be cautious when using with tubing and frits; room temperature only. B Stainless Steel Picric acid B Stainless Steel Potassium bichromate B Stainless Steel Phosphoric acid 10% Chemical Compatibility Chart (continued on page 61) 60 Chemical Compatibility Chart | MiDas™ Substance Fraction Severity Material Notes Subject to pitting. Potassium bromide B Stainless Steel Potassium carbonate B Stainless Steel Potassium chloride 10% B Stainless Steel Potassium ferricyanide 10% B Stainless Steel Potassium ferrocyanide 10% B Stainless Steel Potassium hydroxide 10% B Stainless Steel (C @ 100%) Potassium nitrate 100% B Stainless Steel Elevated temperatures may reduce resistance. B Stainless Steel B Stainless Steel Potassium sulfide B Stainless Steel Pseudocumene B UHMWPE Pyrogallic acid B Stainless Steel Quinine Bisulfate B Stainless Steel Quinine sulfate B Stainless Steel Rosin B Stainless Steel Silver chloride C Stainless Steel Silver nitrate B Stainless Steel Sodium (hot) C PEEK Sodium acetate B Stainless Steel Potassium oxalate Potassium permanganate 10% Sodium carbonate 10% B Stainless Steel Sodium chloride 10% B Stainless Steel Sodium chlorite Bleach 50% B UHMWPE Sodium hyposulfite 100% B Stainless Steel Sodium nitrate 50% B Stainless Steel Chemical Compatibility Chart Chemical Compatibility Chart Elevated temperatures may reduce resistance. Chemical Compatibility Chart (continued on page 62) MiDas™ | User’s Guide 61 Chemical Compatibility Chart Chemical Compatibility Chart Substance Fraction Sodium peroxide Severity Material Notes B UHMWPE Room temperature only. Sodium sulfate 20% B Stainless Steel Sodium sulfide 50% B Stainless Steel Stannic chloride C Stainless Steel Stearic acid B Stainless Steel Sulfur chloride B Stainless Steel Sulfur dioxide 100% B Stainless Steel Sulfur trioxide 10% C UHMWPE Sulfuric acid > 40% conc. B PEEK Prolonged exposure may cause deterioration. (C @ 100%) Sulfuric acid (aerated) B Stainless Steel Elevated temperatures may reduce resistance. Sulfuric acid (air free) B Stainless Steel Elevated temperatures may reduce resistance. B Stainless Steel C UHMWPE Sulfurous acid 100% Sulfuryl chloride Room temperature only. Tanic acid 100% B Stainless Steel Tartaric acid 50% B Stainless Steel Tetrabromoethane B UHMWPE Elevated temperatures and prolonged exposure may reduce resistance. Tetrahydrofuran (THF) A PEEK Be cautious when using with tubing and frits; room temperature only. Not recommended for use with PEEK rotor seals. Tetrahydrofuran (THF) B PCTFE Thionyl chloride C UHMWPE Thionyl chloride B PCTFE Thiophene B UHMWPE Room temperature only. Chemical Compatibility Chart (continued on page 63) 62 Chemical Compatibility Chart | MiDas™ Substance Fraction Severity Material Notes Elevated temperatures may reduce resistance. Toluene B UHMWPE Trichlorethylene B Stainless Steel Trifluoromethyl sulfonic acid C Xylene (p-) B PEEK UHMWPE Elevated temperatures may reduce resistance. MiDas™ | User’s Guide Chemical Compatibility Chart Chemical Compatibility Chart 63 C Appropriate Delivery Rates Appendix C At low attenuation, hence high attenuator frequency, sample has to be supplied at a higher rate to fill the rotor groove on each cycle. If this is not ensured, then a higher attenuation than expected is observed. Refer to the table below when selecting the delivery rate. Recommended Minimum Delivery Rate for Various Attenuation Levels Attenuation at 0.5 mL/min Make-up Pump Rate Attenuation at 1 mL/min Make-up Pump Rate Attenuation at 2 mL/min Make-up Pump Rate Minimum required delivery rate (µL/min) 1669 3337 6675 50 1250 2500 5001 50 984 1968 3935 50 833 1665 3330 50 681 1363 2725 50 644 1288 2577 50 493 985 1970 50 341 682 1364 50 265 530 1060 50 189 379 758 50 167 333 667 100 133 267 533 100 125 250 500 100 100 200 400 100 83 167 333 100 Recommended Minimum Delivery Rate for Various Attenuation Levels Table (continued on page 66) MiDas™ | User’s Guide 65 Appropriate Delivery Rates Recommended Minimum Delivery Rate for Various Attenuation Levels Attenuation at 0.5 mL/min Make-up Pump Rate Attenuation at 1 mL/min Make-up Pump Rate Attenuation at 2 mL/min Make-up Pump Rate Minimum required delivery rate (µL/min) 67 133 267 100 50 100 200 100 42 83 167 100 33 67 133 200 25 50 100 200 19 39 78 200 17 33 67 200 13 25 50 200 In Direct Sampling, a fixed volume of sample is being delivered to attenuator. This will be analyzed by the VERITY® 1900 MS Detector over a number of scans obtained from the following relation: Scans = 60 ∙ Vloop Ft Where F is the delivery rate (in µL/min) and t is the scan time (in seconds). It is recommended that analysis is performed over at least 10 scans for reproducible results. 66 Appropriate Delivery Rates | MiDas™