flexar solvent manager users and service guide.pdf

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FLEXAR SOLVENT M ANAGER

User’s and Service Guide

LIQUID CHROMATOGRAPHY



Release History

Part Number Release Publication Date

09936949 A June 2009

Any comments about the documentation for this product should be addressed to:

User AssistancePerkinElmer710 Bridgeport AvenueShelton, CT 06484-4794U.S.A.

Or emailed to: [email protected]

NoticesThe information contained in this document is subject to change without notice.Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes nowarranty of any kind with regard to this document, including, but not limited to, theimplied warranties of merchantability and fitness for a particular purpose.

PerkinElmer shall not be liable for errors contained herein for incidental consequential damages inconnection with furnishing, performance or use of this material.

Copyright InformationThis document contains proprietary information that is protected by copyright.

All rights are reserved. No part of this publication may be reproduced in any form whatsoever ortranslated into any language without the prior, written permission of PerkinElmer, Inc.

Copyright © 2009 PerkinElmer, Inc.

TrademarksRegistered names, trademarks, etc. used in this document, even when not specifically marked as such,are protected by law.

PerkinElmer is a registered trademark of PerkinElmer, Inc.



Long-Term Shutdown .....................................................................41

Maintenance....................................................................................43

Preventive Maintenance..................................................................45

Troubleshooting Guide ..........................................................................46

Index...................................................................................................47



Introduction



6 . Flexar Solvent Manager



Overview

The Flexar Solvent Manager, with a 3-CH vacuum degasser or 5-CH vacuum degasser, providessafe and convenient management of LC solvent bottles. A removable bottle tray can hold up totwo 2L and three 1L solvent bottles. The Flexar Solvent Manager with 3-CH vacuum degassingincludes two 1L and one 500mL bottles, fitted with caps, tubing and 10 μm filter frits. The Flexar

Solvent Manager with 5-CH vacuum degassing includes two 2L , one 1L, and one 500mL bottles,fitted with caps, tubing and 10 μm filter frits. An easily-removable magnetized front panelprovides immediate access to enclosed compartment which can be used to hold an LC column.There is also a rear compartment for housing either dotLINK or Ethernet communicationdevices.

Ergonomic design includes integrated 3-channel, or 5-channel vacuum degassing unit. Allsolvent lines conveniently managed through rear manifold.

There are tube management clips integrated into all four corners of the pump front fasciaassure secure tubing positioning while allowing flexibility in tubing configuration. Anintegrated drain tray and inter-component drain management also built into front fasciaprovide protection against leaks – drain management designed for plug-and-play with allother Flexar components. Color-coded LED display indication for power, system status anddegasser vacuum.



Introduction . 9

About This Manual

This guide is divided into following chapters:

Chapter 1 Introduction

This chapter contains a brief introduction on the instrument, the conventions and warningsused in the manual.

Chapter 2 Safety Practices

Important safety information is provided in this chapter.

Chapter 3 Description

This chapter contains information on the components of the instrument, how it works andinstrument specifications.

Chapter 4 Installation

Information on installing and re-installing your instrument should you ever need to moveyour system is provided.

Chapter 5 Maintenance

Maintenance and cleaning procedures for the various components of your instrument areprovided.



Introduction . 11

CAUTION We use the term CAUTION to inform you about situations that couldresult in serious damage to the instrument or other equipment.Details about these circumstances are in a box like this one.

D Caution (Achtung)

Bedeutet, daß die genannte Anleitung genau befolgt werden muß, umeinen Geräteschaden zu vermeiden.

DK Caution (Bemærk)

Dette betyder, at den nævnte vejledning skal overholdes nøje for atundgå en beskadigelse af apparatet.

E Caution (Advertencia)

Utilizamos el término CAUTION (ADVERTENCIA) para advertir sobresituaciones que pueden provocar averías graves en este equipo o enotros. En recuadros éste se proporciona información sobre este tipo decircunstancias.

F Caution (Attention)

Nous utilisons le terme CAUTION (ATTENTION) pour signaler lessituations susceptibles de provoquer de graves détériorations del'instrument ou d'autre matériel. Les détails sur ces circonstancesfigurent dans un encadré semblable à celui-ci.

I Caution (Attenzione)

Con il termine CAUTION (ATTENZIONE) vengono segnalate situazioniche potrebbero arrecare gravi danni allo strumento o ad altraapparecchiatura. Troverete informazioni su tali circostanze in un riquadrocome questo.

NL Caution (Opgelet)

Betekent dat de genoemde handleiding nauwkeurig moet worden

opgevolgd, om beschadiging van het instrument te voorkomen.

P Caution (Atenção)

Significa que a instrução referida tem de ser respeitada para evitar adanificação do aparelho.




WARNING

We use the term WARNING to inform you about situations that couldresult in personal injury to yourself or other persons. Details aboutthese circumstances are in a box like this one.

D Warning (Warnung)

Bedeutet, daß es bei Nichtbeachten der genannten Anweisung zu

einer Verletzung des Benutzers kommen kann.

DK Warning (Advarsel)

Betyder, at brugeren kan blive kvæstet, hvis anvisningen ikkeoverholdes.

E Warning (Peligro)

Utilizamos el término WARNING (PELIGRO) para informarle sobresituaciones que pueden provocar daños personales a usted o aotras personas. En los recuadros como éste se proporcionainformación sobre este tipo de circunstancias.

F Warning (Danger)

Nous utilisons la formule WARNING (DANGER) pour avertir dessituations pouvant occasionner des dommages corporels àl'utilisateur ou à d'autres personnes. Les détails sur ces circonstancessont données dans un encadré semblable à celui-ci.

I Warning (Pericolo)

Con il termine WARNING (PERICOLO) vengono segnalate situazioniche potrebbero provocare incidenti alle persone. Trovereteinformazioni su tali circostanze in un riquadro come questo.

NL Warning (Waarschuwing)

Betekent dat, wanneer de genoemde aanwijzing niet in acht wordtgenomen, dit kan leiden tot verwondingen van de gebruiker.

P Warning (Aviso)Significa que a não observância da instrução referida poderá causarum ferimento ao usuário.



Safety Practices



Safety Practices . 15

Overview

This chapter describes the general safety practices and precautions that must be observedwhen operating the Flexar Solvent Manager.

This advice is intended to supplement, not supersede, the normal safety codes in the user'scountry. It is also a supplement to the PerkinElmer standard Safety and Health Policy. Theinformation provided does not cover every safety procedure that should be practiced.Ultimately, maintenance of a safe laboratory environment is the responsibility of the analystand the analyst's organization.

Please consult all manuals supplied with the Flexar Solvent Manager and accessories beforeyou start working with the instrument. Carefully read the safety information in this chapterand in the other manuals supplied. When setting up the instrument or performing analyses ormaintenance procedures, strictly follow the instructions provided.

Precautions

WARNING

Be sure that all instrument operators read and understand the precautions listed below. It is advisable to post a copy of the precautions near or on the instrument shelf.

The following precautions must be observed when using the Flexar Solvent Manager:

• Be sure that the voltage of the Flexar Solvent Manager power supply corresponds to thevoltage used in your laboratory.

• Never remove the cover panels from the Flexar Solvent Manager without first shutting itdown and disconnecting the power cord from line power.




General Operating Conditions

Only use the Flexar Solvent Manager indoors in a non-explosive environment and under thefollowing conditions:

Temperature 10 oC to 35 oC

Relative Humidity 20 - 80% (non-condensing)

Altitude up to 2000 m

Environmental Conditions

The instrument has been designed to be safe under the following conditions:

• Indoor use

• Altitude up to 2000 m

• Ambient temperatures of 5 oC to 40 oC

• An ambient relative humidity of 20 - 80% (non-condensing)

• Mains fluctuations not exceeding + 10% of the nominal voltage.

• Pollution degree 2

WARNING

If the equipment is used in a manner not specified herein, the protection provided by the equipment may be impaired.

NEVER operate the instrument in an explosive environment!

Storage Conditions

The instrument may be stored under the following conditions:

• Ambient temperature is –20 to +60 °C

• Ambient relative humidity is 20 to 80% (non-condensing)

• Altitude is in the range 0 to 12 000 m




Electrical Safety

The instrument has been designed to protect the operator from potential electrical hazards.This section describes some recommended electrical safety practices.

The instrument must be correctly connected to a suitable electrical supply.

When working with the instrument observe the following:

• Be sure to use the correct plug adapter on the power supply for your laboratory.

• The instrument is to be positioned in a clean area free of dust, smoke, vibration, andcorrosive fumes, out of direct sunlight, and away from heating or cooling units or ducts.

• Do not attempt to make adjustments, replacements or repairs to this instrument exceptas described in the accompanying User Documentation. Only a PerkinElmer servicerepresentative or similarly trained and authorized person should be permitted to servicethe instrument.

• Whenever it is possible that the instrument is no longer electrically safe for use, makethe instrument inoperative and secure it against any unauthorized or unintentional

operation. The electrical safety of the instrument is likely to be impaired if, for example,the instrument shows visible damage; has been subjected to prolonged storage underunfavorable conditions; or has been subjected to severe stress during transportation.




WEEE Instructions for PerkinElmer Products

or

A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that theproduct is covered by the Waste Electrical and Electronic Equipment (WEEE) Directive and isnot to be disposed of as unsorted municipal waste. Any products marked with this symbolmust be collected separately, according to the regulatory guidelines in your area.

The objectives of this program are to preserve, protect and improve the quality of theenvironment, protect human health, and utilize natural resources prudently and rationally.

Specific treatment of WEEE is indispensable in order to avoid the dispersion of pollutants intothe recycled material or waste stream. Such treatment is the most effective means ofprotecting the customer’s environment.

Requirements for waste collection, reuse, recycling, and recovery programs vary byregulatory authority at your location. Contact your local responsible body (e.g., yourlaboratory manager) or authorized representative for information regarding applicabledisposal regulations. Contact PerkinElmer at the web site listed below for information specificto PerkinElmer products.

Web address:

http://las.perkinelmer.com/OneSource/Environmental-directives.htm

For Customer Care telephone numbers select “Contact us” on the web page.

Products from other manufacturers may also form a part of your PerkinElmer system. Theseother producers are directly responsible for the collection and processing of their own wasteproducts under the terms of the WEEE Directive. Please contact these producers directlybefore discarding any of their products.

Consult the PerkinElmer web site (above) for producer names and web addresses.






Decontamination and Cleaning

Before using any cleaning or decontamination methods except those specified byPerkinElmer, users should check with PerkinElmer that the proposed method will not damagethe equipment.

DecontaminationCustomers wishing to return instrumentation and/or associated materials toPerkinElmer for repair, maintenance, warranty or trade-in purposes are advisedthat all returned goods must be certified as clean and free from contamination.

The customer’s responsible body is required to follow the "Equipment DecontaminationProcedure" and complete the “Certificate of Decontamination”. These documents areavailable on the PerkinElmer public website:

http://las.perkinelmer.com/OneSource/decontamination.htm

If you do not have access to the internet and are located in the U.S., call toll free at 1-800-

762-4000 or (+1) 203-925-4602, 8:30 a.m. – 7 p.m. EST and speak to CustomerSupport.

In Canada, call toll free 800-561-4646 and speak to Customer Support.

If you are located outside of the United States or Canada, please call your local PerkinElmersales office for more information.

Cleaning the Instrument

Exterior surfaces may be cleaned with a soft cloth, dampened with a mild detergent andwater solution. Do not use abrasive cleaners or solvents.






ElectroMagnetic Compatibility (EMC)

Europe

All information concerning EMC standards is in the Declaration of Conformity, and thesestandards may change as the European Union adds new requirements.

PerkinElmer instruments have been designed and manufactured, having regard to the stateof the art, to ensure that:

a. the electromagnetic disturbance generated does not exceed the level above which radioand telecommunications equipment or other equipment cannot operate as intended;

b. it has a level of immunity to the electromagnetic disturbance to be expected in itsintended use which allows it to operate without unacceptable degradation of its intendeduse.

Labels on Instrument




Quality Control/Good Laboratory Practices

The user should develop appropriate quality control procedures for the instrument to ensuresuitability for its intended use. These procedures typically consist of periodic performanceverifications and routine inspections and suitability tests.

Certificate of System ControlEach instrument is carefully built and tested in a controlled system in accordance with therequirements specified in its applicable PerkinElmer Final Assembly and Test Specification.

Each instrument is certified to meet its functional and performance specification upon releaseto shipment. The integrity of this quality system is routinely audited and certified.

Hazardous Chemicals

Before using mobile phase solvents, you should be thoroughly familiar with all hazards andsafe handling practices. Observe the manufacturer’s recommendations for use, storage anddisposal. These recommendations are normally provided in the material safety data sheets(MSDS) supplied with the solvents.

WARNING

Some chemicals used with this instrument may be hazardous or maybecome hazardous after completion of an analysis. The responsible body(e.g., Lab Manager) must take the necessary precautions to ensure thatthe surrounding workplace and instrument operators are not exposed tohazardous levels of toxic substances (chemical or biological) as definedin the applicable Material Safety Data Sheets (MSDS) or OSHA, ACGIH,or COSHH documents. Venting for fumes and disposal of waste must bein accordance with all national, state and local health and safetyregulations and laws.

Definitions in Warning for Hazardous Chemicals

Responsible body: “Individual or group responsible for the use and maintenance ofequipment, and for ensuring that operators are adequatelytrained.” [per IEC 61010-1]

Operator: “Person operating equipment for its intended purpose.” [per IEC61010-1, ]

OSHA: Occupational Safety and Health Administration (United States)

ACGIH: American Conference of Governmental Industrial Hygienists

COSHH: Control of Substances Hazardous to Health (United Kingdom)




Safe Handling of Solvents

WARNING

Give careful attention to the hazards associated with thesolvents you are using. Refer to the safety data sheets

provided by the manufacturer. For example, Material SafetyData Sheets (MSDS) in the USA.

WARNING

Do not use the Solvent Manager to degas perfluorinatedsolvents. Teflon AF® is soluble in solvents such as theFluorinert series from 3M company and PF series from

Ausimont. Where there is a question about using a particularsolvent that is fluorinated, contact a PerkinElmerrepresentative.

• Wear appropriate eye protection at all times when handling chemicals. Use safetyglasses with side shields, goggles, or full-face shields, according to the types ofchemicals you will be handling.

• Wear suitable protective clothing, including gloves that are specifically resistant to thechemicals being handled.

• Always use clean solvents. Solvents which have been distilled in glass (HPLC Grade) arerecommended.

• Filter the solvents and buffers through a 0.5-micron medium as an additionalprecaution.

• Degas all aqueous and most organic solvents prior to use.

• Store flammable solvents or solvents which may form hazardous by-products when theinstrument is shut down, by following the recommended shutdown procedure.

• Check compatibility of solvent(s) with the type of column(s) being used.

• Know the relative polarity and miscibility of the solvents being used.

Solvents with Low Boiling Points

Do not use liquids that have a boiling point less than 30 °C.

WARNING

Do not use carbon disulfide or other solvents which have an

auto-ignition temperature below 110 °C.




Buffers

Exercise care when using buffers in conjunction with organic solvents. NEVER LEAVEBUFFERS IN THE SYSTEM OVERNIGHT. Buffers left in the system can form salt crystalswhich may cause premature injector valve failure and plug the transfer tubing and sampleneedle. To remove buffers, flush the system with water followed by methanol or isopropanol.Remember to change the flush solvent from methanol or isopropanol to water before usingbuffers.

Corrosion

The following corrosion precautions apply to the standard (stainless steel) and thebiocompatible (titanium) instruments.

All parts of the instrument that contact mobile phase are made of stainless steel, KelF, andquartz. Some of these materials are extremely sensitive to acid chlorides. If you havequestions about your mobile phase or flush solvent, contact a PerkinElmer representative.Refer to the table below.

Solvents Which May Corrode an LC Instrument

Aqua Regia (80% HCl, 20% HNO3)Hydrogen Peroxide

Anhydrous ChlorideDichloromethaneSulfuric Acid (Conc.)Hydrochloric Acid (20% and 37%)Hydrofluoric Acid (20%, 50%, and 75%)Copper Chloride

BromineFreon 12 (wet)Chlorinated solventsHydrofluorosilicic Acid (20%)Hydrobromic Acid (20%)Ferric ChlorideFerrous ChlorideMercuric Chloride (Dilute)

If you have questions about your mobile phase, contact a PerkinElmer representative. Referto the table below:

WARNING

Aqua Regia and sulfuric acid are known to dissolve titanium.

Solvents with Auto-Ignition Temperature Below 110 °C

Certain solvents have a temperature at which they are combustible upon contact with aheated surface, even in the absence of a spark or other source of ignition. A list of common

solvents with their auto-ignition temperatures is shown below.

WARNING

Do not use carbon disulfide or other solvents which have an auto- ignition temperature below 110 °C.




Auto-Ignition Temperatures of Common LC Solvents.

Solvent Auto-IgnitionTemperature (°C)

Carbon Disulfide 100

Diethyl Ether 180

Cyclohexane 260Hexane 261

Petroleum Ether (naphtha) 288

Pentane 309

Tetrahydrofuran 321

Dioxane 366

Propanol 404

iso-Octane 418

Ethanol 423

Isopropyl Ether 443

Dimethylformamide 445

Methanol 446

Isopropanol 455

Methylethylketone 474

Acetonitrile 524

Ethyl Acetate 524

Toluene 536

Acetone 538

Benzene 562

Air Bubbles

To prevent air from entering the system, and to ensure that pressure fluctuations do notoccur, observe the following precautions:

• Ensure that the pump's solvent inlet filter is below the solvent level in the solventreservoir.

• If the pump has not been used for an extended period of time, remove air bubbles byconnecting a priming syringe to the drain valve on the pump, opening the drain valve,

and fast-flushing the system to prime the pump. After priming the pump, close thedrain valve completely.

• If bubbles are observed in the flow cell, degas the solvent and add back-pressure deviceP/N 09907126.



Description



Description . 27

Overview

The Solvent Manager is a high-efficiency in-line module that removes dissolved gasses fromHPLC solvents. Its unique design assures reliable continuous operation and the highest levelof continuous performance available without the need for helium degassing. Up to fivesolvent lines may be degassed simultaneously by one unit. The extremely low internalvolume of each Teflon AF® channel offers very quick equilibration and very short startuptimes compared with PTFE degassing channels which have the same degassing efficiency.

Inside the unit, the solvent flows through a short length of Teflon AF® tubing which islocated in a vacuum chamber. Within this chamber a partial vacuum is maintained by aconstantly running, low RPM vacuum pump. Dissolved gasses migrate across the tubing wallunder a concentration gradient produced by the vacuum as the solvent flows within the coil.Gasses removed are expelled, and the chamber is maintained at a constant, preset vacuumlevel by varying the vacuum pump speed as needed.

A special port in the vacuum pump continually flushes the pump head with a small “bleed” ofair to remove any solvent vapors which may enter the pump from the vacuum chamber. Thisair bleed eliminates the need for any solenoid valves within the system. This patented*

design results in zero vacuum “hysteresis”. Previous designs allowed the vacuum chamberpressure to fluctuate, with the pump cycling on and then off in response to the vacuum level.

How the Vacuum Degasser Operates

Immediately upon turning on the instrument, the microprocessor examines the vacuumsensor signal to confirm that it is within an expected range. Following the startup test, themicroprocessor ramps the vacuum pump to high RPM, to quickly exhaust atmosphere fromthe vacuum chamber. As the vacuum level approaches the preset control value, the pumpRPM will slowly ramp down to a low speed (typically 40 to 60 RPM). Afterwards, the pumpRPM will vary slightly, as needed under the changing degassing load, to maintain a virtuallyconstant vacuum level (50 ±0.5 mm Hg). This "zero hysteresis, constant run" (ZHCR ®)mode is necessary, due to the extremely low mass, high response, Teflon AF® degassingtubing. Only a ZHCR ® design ensures a baseline which is unaffected by the degasser.




Solvent Manager Status LEDs

The Flexar Solvent Manager status is displayed on the front panel through the followingindicator lights.

LED Functionality

Power On LED Instrument StatusOFF OFF

ON (green) ON

Ready/Error LED Instrument Status

OFF OFF

ON (green) Ready/Running – No Error

ON (red) Error

Vacuum LED Instrument Status

OFF OFF

ON (green) At vacuum

ON (red) Not to vacuum

Power OnLED

Ready/ErrorLED

VacuumLED

Green Green/Red Green/Red



Description . 29

Principles of Operation

The Flexar Solvent Manager vacuum degasser consists of a vacuum chamber, degassingtube, variable speed vacuum pump, microprocessor controller, sensor, and check valves. Thesolvent (mobile phase) flows into a degassing tube, which is inside a vacuum chamber.Decreased pressure in the chamber causes the outward movement of gas dissolved in themobile phase across the tube wall, in accordance to Henry’s Law, thus degassing the mobile

phase. The pressure in the vacuum chamber is established by the vacuum pump andmonitored by the microprocessor through an integrated absolute pressure sensor. Degassedmobile phase exits the vacuum degasser and enters the pump.

Figure 1 Schematic of the 5-Channel Solvent Manager vacuum degasser

Smart Leak Detection An additional benefit of maintaining a constant vacuum level is that a potential leak in thevacuum degassing system can be observed by monitoring the RPM of the pump. This “smartleak detection” is a benefit of the patented design of the degasser. If a leak occurs withinthe chamber, the microprocessor will increase the pump RPM in an attempt to maintain thevacuum level. If the pump cannot maintain the vacuum level (if it runs at an elevated RPMfor more than 2 minutes), the red LED will flash, indicating a possible leak condition, and thesystem will shut down and go into a safe mode.

Principles of degassing using Teflon AF ® membranes

This relatively recent addition to the field of degassing has properties not found in otherfluoropolymers. The fully amorphous nature of this fluoropolymer and its molecular structurecreates a molecular level porosity unlike the mechanically induced porosity in PTFE extrudedtubing. In addition, unlike the process used in extruding PTFE, no extrusion agents areneeded (like kerosene, etc.) which contaminate mobile phases until they are extracted by themobile phase over time. Likewise, this molecular structure, combined with the very smallsurface areas required to degas the mobile phase, reduces the possibility of carryover fromone solvent or mobile phase to another to virtually zero.




Teflon AF® is so non-polar that it is both solvophobic and hydrophobic. This feature of Teflon AF® reduces the possibility of cross-channel contamination from one channel to another, andwhen combined with the ultra-low internal volumes of Teflon AF® channels needed for HPLCflow rates, all but eliminates this cross contamination concern by the chromatographer.Teflon AF® has been used in certain optical systems associated with HPLC for a few yearswithout concern for normal HPLC solvents. However, Teflon AF® is soluble in certainsolvents (see cautionary statements) and must not be used to degas these types of solvents.

Teflon AF

®

is permeable to some degree to water vapor whereas PTFE is not. While thevacuum pump in the vacuum degasser contains internal provisions for sweeping water orsolvent vapor from the pump continuously, it is possible that over time, high concentrationbuffers may form crystals within the channel due to the loss of water within the channel. Thesame precautions should be taken to prevent crystallization within these channels as aretaken for the HPLC pump. See the “Short-term Shutdown” procedures.

Vacuum Degasser Performance

The following graph illustrates the performance of the vacuum degasser.



Description . 31

Specifications

Specification Description

Channels 3-channel version or 5-channel versionDegassing Process Gas permeation through a fluoropolymer membrane

Maximum Recommended FlowRate1

3.0 mL/min.

Pressure Drop2 1.37 mm Hg/mL/min.Degassing Capacity ~25% dissolved gases remaining in 60:40 MeOH/Water

mixture at 1 mL/min.Dead Volume ~480 microliters per channel for standard channelMaterials contacting solvents PEEK, Glass-filled PTFE, Teflon AF®

Power:

Power requirement 100 to 240 VAC (±10%), 1A, 47 to 63 HzPower Supply Adapter Plugs 4 supplied with power supply, interchangeable: North

America/Japan, U.K., Continental Europe, AustraliaInstallation Over-Voltage Category II

Validation Output:Signal 5 mVDC / 1 mm Hg absolute from 20 to 800 mm Hg

(0.100 VDC at 20 mm Hg; 4.000 VDC at 800 mm Hg) Accuracy ±1.0% of reading ±0.010 VDC from 20 to 800 mm Hg

Operating Conditions:

Ambient Temperature 10 to 35 ºC Ambient Relative Humidity (RH) 20 to 80 % RH (without condensation) Altitude 0 to 2000 MetersIndoor vs. Outdoor Use IndoorPollution Degree 2

Storage Conditions:

Ambient temperature -20 to +60 ºC

Ambient Relative Humidity 20 to 80% RH (without condensation) Altitude 0 to 12000 M

1 Maximum recommended flow rate to prevent a 60:40 MeOH/Water mixture from outgassing. The estimateassumes low pressure mixing and low flow restriction prior to the HPLC pump. MeOH/Water mixing representsthe worst outgassing case and maximum flow rate will likely increase with Acetonitrile/Water mixtures. Highpressure mixing will also increase the maximum flow rate. Degassing is still recommended.

2 Calculated tubing pressure per unit change in flow assuming laminar flow with a viscosity of 1.0 cP. Inlet andoutlet bulkheads may contribute to the overall pressure, but are not included in the estimate.



Installation



Installation . 35

Preparing Your Laboratory

Before installing your Solvent Manager, prepare your laboratory according to the following guidelines:

WARNING

Solvent vapor levels that are high enough to interfere with thedetector performance should be considered hazardous tosomeone who is continuously exposed to the vapors.

Adequate Bench Space

Provide bench or table space to accommodate the dimensions of the pump, the detector, and otherinstruments in the system. Provide space at the rear of the instruments for air circulation.

Solvents/Mobile Phase

Use only HPLC grade solvents in all analyses. HPLC grade water and methanol (1 liter each) are requiredfor performance verification.

Waste-Solvent Disposal

Provide a properly labeled chemical waste container in a safe and vented place. Make sure that it iswithin all of the specified safety requirements for your location. Wear gloves, eye protection, and alaboratory coat when handling or disposing of chemical waste.

Electrical Requirements

The AC power supply supplied with the vacuum degasser incorporates a universal AC input, switchingregulator. This allows the instrument to operate at any AC line voltage from 100 to 240 VAC (±10%)with a line frequency range of 47 to 63 Hz. The switching regulator senses the incoming line voltage andautomatically adjusts its operation accordingly. The switching regulator assembly incorporates its ownon-board line voltage fuse. This fuse is not user serviceable. In the event that this fuse blows, it will benecessary to replace the AC power supply.

A set of four interchangeable wall plugs are included to allow the AC power supply to be plugged into thestandard electrical sockets in North America, Japan, the U.K., most countries in continental Europe, and Australia. Plug the female plug into the rear panel power jack. See the figure below.

Figure 2 Rear Panel Power Connector

NOTE: The RS232 connector is not used at this time and reserved for future use.




Unpacking

CAUTION

Take great care when installing your Solvent Manager, andfollow the procedures described in this manual. If you requireassistance, contact your local PerkinElmer Service Engineer.

Carefully unpack the Flexar Solvent Manager and check for obvious signs of damage that may haveoccurred during shipment. Immediately report any damaged or missing items to the shipping carrier andPerkinElmer.

A Start-Up Kit is supplied with the Flexar Solvent Manager containing the following:

Item Quantity

AC Power Supply (including cord and

interchangeable Wall Plugs)P/N N2602390

1

4(North America/Japan, U.K., Continental Europe, Australia)

User’s Guide on CD 1

Port Plug, ¼-28, Rheodyne 6118 2

Installing the AC Power Supply

Locate the AC power supply with attached DC power cord and the set of four interchangeable wall plugs.

Plug the round connector at the end of the cord into the Power jack on the vacuum degasser rear panel.From the set of four plugs, select the one appropriate for the local electrical socket and install it onto the AC power supply. Insert power supply plug into the AC supply. The AC power supply should bepositioned for easy disconnection.

Connecting the Solvent Manager in a Typical System

The following illustration shows the tubing connections that are typically made between the 5-channelvacuum degasser and other instruments in an LC system. The direction of flow through the vacuumdegasser is not critical.

If you have a 3-channel vacuum degasser you will use channel A and B for solvents and channel C for the

autosampler wash solvent.



Installation . 37

Solvent A Solvent B Solvent C Solvent D

HPLCPump

Autosampler

Wash

Auto-Sampler

Solvent Manager

A

BC

D

E

Figure 3 System Tubing Connections

Installing the Solvent Manager

Remove the Solvent Manager from its shipping container and install it by following this procedure:

1. Place the Solvent Manager on top of your Flexar stack.

Examples are shown below:

2. Remove the solvent reservoir bottles from their boxes.

The Flexar Solvent Manager and Flexar Solvent Manager with 3-CH vacuum degassing

includes two 1L and one 500mL bottles, fitted with caps, tubing and 10 μm filter frits.The Flexar Solvent Manager with 5-CH vacuum degassing includes two 2L , two 1L, and one500mL bottles, fitted with caps, tubing and 10 μm filter frits.

3. Remove the storage caps from each bottle and replace them with the blue caps fitted with tubing.

4. Looking at the rear of the Solvent Manager (this example shows a 3-channel degasser) connecttubing from each bottle to channel A and B on the top row of the solvent connectors to each




corresponding bottle. Use channel C for your autosampler wash solvent. Tighten the fitting fingertight to make a leak-free connection.

5. Connect the tubing from each channel (A, B, C) on the bottom row to the corresponding pumpinlets. Tighten the fitting finger tight to make a leak-free connection.

For example, channel A on the pump connects to the lower A connector on the Solvent Manager. Theupper channel A connector on the Solvent Manager connects to the solvent bottle for channel A.

To make a tubing connection:

1. Run a line of 1/8” O.D. x 1/16” I.D. Teflon chromatography tubing from the solvent supply to thevacuum degasser.

2. Push the tubing through a PEEK 1/8” male ¼-28 fitting and slide a ferrule over the tubing end (seefigure below). Cut the Teflon tubing so the end is flat.

3. Screw the ¼-28 fitting into one port on the front of the vacuum degasser (Channel A, for example).The direction of flow through the vacuum degasser is not critical. Plastic connectors should betightened by hand. Overtightening them will damage the threads.

4. Repeat steps 1 through 3 to connect additional lines to be degassed.

5. Once all desired solvent lines have been connected to the vacuum degasser, any and all unusedports should be plugged. Use the plugs supplied. Press each in by hand.

6. Prime each degassing membrane by pulling the solvent from the reservoir through the degassing

system. This can be done by connecting a syringe to the tubing or LC pump priming port anddrawing air and/or mobile phase into the syringe until no air remains in the tubing, approximately5 milliliters.



Installation . 39

CAUTION

DO NOT prime the membranes by pushing solvent through thedegassing systems. This technique can generate several hundred

pounds of pressure which might rupture the membrane, even thoughthe Teflon AF ® membrane is quite rugged. The maximumrecommended pressure on the membrane is 1 mPa (100 psig, 7 Bar).

Operating Summary

The following steps summarize how to use the vacuum degasser:

1. Select and fill each solvent reservoir with the mobile phase for your analysis.

2. Verify that the Flexar Solvent Manager vacuum degasser is properly installed as described.

CAUTION Never connect the Flexar Solvent Manager vacuum degasser tothe output side of the pump. The high pressure may cause

permanent damage to the degassing membrane.

3. Verify that the tubing to your injector, column, and detector is properly connected. Also verify thatplugs are installed in the unused ports.

4. Disconnect and remove the tubing that is connected to the output port (the lower row ofconnectors), connect the priming syringe to this port, and pull the solvent through the degasseruntil bubbles no longer appear. Then reconnect the tubing to the output port.

5. Start solvent flow through the system and check for leaks around the ¼-28 connectors.If a leak occurs at the connection, tighten the fitting an additional 1/8 turn. If the leak persists,disconnect the leaking fitting and inspect it. If the nut and ferrule appear to be in good condition,reconnect the fitting. If the leak persists, replace the nut and ferrule and repeat the procedure untilyou achieve leak-free operation.

The vacuum degasser maintains a constant vacuum pressure of 50 mm Hg absolute (nominal) byvarying the speed of the vacuum pump as needed depending on the degassing load in the system.The pump is designed for at least 5 years of constant running and has integral in-pump venting,which eliminates the need for stop-start running (U.S. Patent 6,248,157). The vacuum level andpump speed is constantly monitored by the microprocessor for changes in operating conditionswhich might be attributed to chamber internal leaks. If a potential leak is detected, the pump willbe shut down and the Status LED will flash. The vacuum is maintained as long as the vacuum

degasser is powered on. Solvent flowing through the vacuum degasser will continue to be degassedso long as the instrument is on and running.

6. Turn on the vacuum degasser by inserting the female plug on the power supply cord into the powerconnector on the rear of the vacuum degasser and start the pump at 1.0 mL/min.




Allow the system to equilibrate for 5-10 minutes. The small volumes contained in the Flexar SolventManager vacuum degasser should only be considered in chromatograph equilibration time whenflow rates less than 1 mL/min are used.

Immediately upon turning on the vacuum degasser, the microprocessor examines the vacuumsensor signal to confirm that it is within an expected range. Following the startup test, themicroprocessor ramps the vacuum pump to high RPM, to quickly exhaust atmosphere from thevacuum chamber. As the vacuum level approaches the preset control value, the pump RPM willslowly ramp down to a low speed (typically 40 to 60 RPM) and will vary slightly as needed under thechanging degassing load to maintain a virtually constant vacuum level.

During initial pump-down, the Status LED will be lit. Once the vacuum has reached normal

operating level, the green Vacuum LED will illuminate. If you want to confirm that the pump isrunning, beyond the front panel LEDs, the slight vibration caused by the microstepping of the motordriving the vacuum pump may be felt by placing your hand on the instrument.

NOTE: Turn off the vacuum degasser by unplugging it from the AC power when the LC to which it is connectedis not in use. The vacuum chamber(s) will slowly return to atmospheric pressure when the unit is powered off. This is accomplished by a small, in-line vacuum bleed and reduces the possibility of solventvapors condensing in the vacuum tubing or pump head.

NOTE: When flushing a line of solvent, the single lumen coil inside the chamber contains a very small amount ofsolvent (approximately 480 microliters). When changing from one solvent to another where the finalsolvent is immiscible with the first, use an intermediate solvent miscible with both the initial and finalsolvent. Carryover from solvent to solvent is much less than previous PTFE designs. Once air bubbles

have been cleared from the solvent line, any further bubbles observed will be coming from the solventreservoir or from a leaking fitting.

NOTE: Since there is virtually no solvent retained within the vacuum degasser (~480 microliters per channel), priming the system is relatively simple. Using the Prime mode on the LC system pump, allow the pumpto draw each solvent to be used in the analysis at a flow rate of 2 mL/min. for 1-2 minutes. This ensuresthat the line from the degasser channel being primed through the proportioning valve on the pump hasfreshly degassed solvent. This dynamic priming method will allow an immediate startup of the analysisupon column equilibration. Contrary to previous PTFE-based degassers, the new vacuum degasser,which uses Teflon AF® membranes, fully degasses solvents within the time it takes for the volume to pass through the chamber, and yet degasses the solvents as thoroughly as, or better than, PTFEchannels containing 40 times more solvent.

Extending the Degassing Flow Rate Range

Certain organic solvents used in reversed phase chromatography outgas upon mixing with water, if notproperly degassed. These solvents are generally alcohols (e.g. methanol), acetonitrile andtetrahydrofuran. Passing water and methanol through a single channel is generally sufficient to degas



Installation . 41

these solvents so outgassing does not occur upon mixing when a 60:40 methanol/water mixture isgenerated by your vacuum degasser or pump at a flow rate of 3 mL/min. If outgassing does occur, or ifa flow rate higher than 3 mL/min. is required, it is a general rule that only the organic portion of themobile phase needs to be passed through a second degassing channel to ensure outgassing does notoccur. This is due to the ability of all organic solvents (e.g. methanol) to hold at least 10 times moredissolved atmosphere than water can.

To more thoroughly degas a mobile phase, connect the outlet of the organic channel to the inlet asecond channel and the outlet of the second channel to the pump. This places the two channels in seriesand doubles the degassing capacity for the organic portion of the mobile phase.

Shutdown

There are two types of shutdown procedures: long-term and short-term.

Short-Term Shutdown (Overnight and Weekends)Observe all precautions pertaining to hazardous solvents and/or those solvents that form harmfuldeposits or by-products.

1. Remove harmful mobile phases from the vacuum degasser and other instruments in the system.

2. Flush the column according to the instructions supplied with the column. Flush buffer salts from thesystem with water. Evaporation leaves salt crystals that may form harmful deposits. Removechloroform or solvents that can decompose to form hydrochloric acid from the system.

CAUTION

Damage caused by precipitating buffer salts in capillary tubing,

or damage resulting from this condition, is specifically excludedfrom warranty.

3. After removing harmful mobile phases, prepare the detector for most mobile phases by flushing itwith isopropanol. To avoid contaminating the system, refilter or discard solvents (including water)that were exposed to the environment for more than 24 hours before use.

4. For weekend storage we recommend flushing 60/40% MeOH/Water through the vacuum degasser,pump, column, and flow cell (provided your column is compatible with MeOH/Water). Then turn offthe vacuum degasser, pump, and detector.

Long-Term Shutdown

1. Follow Short-Term Shutdown procedure Steps 1 and 2.

2. Remove the column and direct the pump output tubing to a beaker. Flush the vacuum degasserfirst with water and then with isopropanol.




3. Turn off the vacuum degasser. Then disconnect the tubing between the vacuum degasser andsolvent reservoirs and the vacuum degasser and pump. Plug all of the ports on the vacuumdegasser.

4. Store the vacuum degasser in a clean, dry location.

5. Before using the vacuum degasser, completely purge it with the correct solvent for the columnbefore reconnecting the column and restarting the system.



Maintenance



44



Maintenance . 45

Preventive Maintenance

Preventive maintenance ensures that your Solvent Manager will perform consistently at anoptimal level. To maintain its optimum operating condition, we recommend the following:

• Adhere to standard laboratory cleanliness practices.

• Use only high-purity solvents (preferably HPLC grade) for mobile phases. (Water should

be bottled HPLC grade, or filtered and deionized.)• Filter the solvents to avoid particulate contamination and tubing blockages.

• Use only high-purity gases when drying contact areas.

• Ensure that all new tubing is passivated and thoroughly flushed before making detectorconnections. (The tubing available from PerkinElmer is passivated.)

• Follow the short- and long-term shutdown procedures.




Troubleshooting Guide

Problem Probable Cause Solution

1) The AC power is plugged in butall 3 LED’s are off, indicating nopower to the degasser.

(a) No AC power at the outlet.

(b) Blown power supply fuse.

(a) Restore power.

(b) Replace the power supply(P/N N2602390).

2) Status LED is on steadily,pump is running and RPM seemshigh.

2) Pump is in initial pull-downphase or system’s degassingdemand has increased.

2) Typically normal operation,although if pump speed continuesto rise for an extended period oftime (as heard by the pitch of thestepper motor) it could indicate apotential fault condition.

3) Status LED is flashingapproximately 1 second off, 1second on. Vacuum pump is notrunning.

3) Possible system leak. 3) Contact your ServiceRepresentative.

4) Status LED is flashingapproximately 2 seconds off, 1second on. Vacuum pump is not

running.

4) Possible sensor or ControlBoard fault.

4) Contact your ServiceRepresentative.

5) Is there a way to checkwhether the system is operatingcorrectly when Power and

Vacuum green LEDs areilluminated, but pump can’t beheard running?

5) Due to the design of the pumpand degasser, the pump isvirtually silent at low RPM, eventhough vacuum is good anddegassing is normal.

5a) Place a hand on the top of theunit. A slight vibration can be feltindicating the pump is operatingat low RPM.

5b) Monitor the UV absorbance ofnon-degassed methanol at 215nM versus degassed methanolcoming through the degasser.Proper performance of thedegasser should decrease the UVabsorbance of the methanolsignificantly.

6) Bubbles appear through theoutput tubing.

6) Loose fitting(s). 6) Tighten the input and outputfittings.

7) No solvent flow. 7a) Air in the HPLC pump head.

7b) If a buffer solvent was left inthe degasser for some time afteruse, it may plug the degasserelements.

7a) Prime/purge the pump head.

7b) Use a different channel, orconnect the channel to a beakerof the solvent without the buffer.Draw the solvent through thechannel to dissolve the buffer.Do not push the solvent throughthe channel. If this flushingaction does not work, contactyour Service Representative.



Maintenance . 47

Index

A

About This Manual ................................................ 9 Air Bubbles..........................................................24

B

Bench Space, providing adequate .........................35Buffers................................................................23

C

ChemicalsDefinitions of Warnings ...................................21Hazardous ......................................................21

Cleaning the Instrument.......................................19Conventions

Notes, cautions and warnings ..........................10text ................................................................10

Corrosion ............................................................23

D

Decontamination .................................................19Degasser Operation .............................................27Degasser Performance .........................................30Degasser Schematics ...........................................29Degassing flow rate range ....................................40

E

Electrical Safety ...................................................17ElectroMagnetic Compatibility ...............................20Environmental Conditions .....................................16

H

HPLC grade solvents ............................................35

I

Installationstart-up kit......................................................36

Instrument Specifications .....................................31

L

Laboratory Practices

GLP ............................................................... 21

O

Operating summary............................................. 39

P

Precautions......................................................... 15Preventive Maintenance....................................... 45Principles of Operation ........................................29

Q

Quality Control.................................................... 21

S

SafetySummary .........................................................8

Safety Information .............................................. 15electrical safety .............................................. 17environmental conditions ................................ 16

Shutdown...........................................................41long-term....................................................... 41short-term ..................................................... 41

Solvents .............................................................22 Auto-Ignition Temperature..............................23Low boiling points ..........................................22

Specifications...................................................... 31Start-up Kit......................................................... 36Storage Conditions.............................................. 16System Description

major components.......................................... 28specifications.................................................. 31

T

Teflon-AF Membranes .........................................29Troubleshooting Guide ........................................ 46

W

WarningsHazardous Chemical ....................................... 21

Waste and Solvent Disposal.................................35WEEE Instructions............................................... 18

flexar solvent manager users and service guide.pdf

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