Você está na página 1de 47

FLEXAR SOLVENT MANAGER

Users 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 Assistance
PerkinElmer
710 Bridgeport Avenue
Shelton, CT 06484-4794
U.S.A.

Or emailed to: info@perkinelmer.com

Notices
The 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 no
warranty of any kind with regard to this document, including, but not limited to, the
implied warranties of merchantability and fitness for a particular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in
connection with furnishing, performance or use of this material.

Copyright Information
This 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 or
translated into any language without the prior, written permission of PerkinElmer, Inc.

Copyright 2009 PerkinElmer, Inc.


Trademarks
Registered 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.

Flexar Solvent Manager . 3
Table of Contents

Table of Contents ...................................................................................3
Introduction......................................................................................5
Overview...............................................................................................7
Safety Summary.....................................................................................8
About This Manual ..................................................................................9
Conventions Used in this Manual............................................................ 10
Notes, Cautions, and Warnings........................................................ 10
Safety Practices ..............................................................................13
Overview............................................................................................. 15
Precautions.......................................................................................... 15
General Operating Conditions ................................................................ 16
Environmental Conditions ............................................................... 16
Storage Conditions......................................................................... 16
Electrical Safety.................................................................................... 17
WEEE Instructions for PerkinElmer Products ........................................... 18
Decontamination and Cleaning............................................................... 19
Decontamination............................................................................ 19
Cleaning the Instrument ................................................................. 19
ElectroMagnetic Compatibility (EMC) ...................................................... 20
Europe.......................................................................................... 20
Labels on Instrument ............................................................................ 20
Quality Control/Good Laboratory Practices .............................................. 21
Certificate of System Control ........................................................... 21
Hazardous Chemicals ..................................................................... 21
Definitions in Warning for Hazardous Chemicals................................ 21
Safe Handling of Solvents...................................................................... 22
Solvents with Low Boiling Points...................................................... 22
Buffers.......................................................................................... 23
Corrosion ...................................................................................... 23
Solvents with Auto-Ignition Temperature Below 110 C..................... 23
Air Bubbles.................................................................................... 24
Description......................................................................................25
Overview............................................................................................. 27
How the Vacuum Degasser Operates ............................................... 27
Solvent Manager Status LEDs ................................................................ 28
LED Functionality ........................................................................... 28
Principles of Operation.......................................................................... 29
Smart Leak Detection ..................................................................... 29
Principles of degassing using Teflon AF

membranes ........................ 29
Vacuum Degasser Performance ............................................................. 30
Specifications ....................................................................................... 31
Installation......................................................................................33
Preparing Your Laboratory..................................................................... 35
Adequate Bench Space................................................................... 35
Solvents/Mobile Phase.................................................................... 35
Waste-Solvent Disposal .................................................................. 35
Electrical Requirements .................................................................. 35
Unpacking............................................................................................ 36
Installing the AC Power Supply .............................................................. 36
Connecting the Solvent Manager in a Typical System............................... 36
Installing the Solvent Manager............................................................... 37
Operating Summary.............................................................................. 39
Extending the Degassing Flow Rate Range....................................... 40
Shutdown ............................................................................................ 41
Short-Term Shutdown (Overnight and Weekends) ............................ 41
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, provides
safe and convenient management of LC solvent bottles. A removable bottle tray can hold up to
two 2L and three 1L solvent bottles. The Flexar Solvent Manager with 3-CH vacuum degassing
includes two 1L and one 500mL bottles, fitted with caps, tubing and 10 m 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 m filter frits. An easily-removable magnetized front panel
provides 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 communication
devices.
Ergonomic design includes integrated 3-channel, or 5-channel vacuum degassing unit. All
solvent lines conveniently managed through rear manifold.
There are tube management clips integrated into all four corners of the pump front fascia
assure secure tubing positioning while allowing flexibility in tubing configuration. An
integrated drain tray and inter-component drain management also built into front fascia
provide protection against leaks drain management designed for plug-and-play with all
other Flexar components. Color-coded LED display indication for power, system status and
degasser vacuum.




8 . Flexar Solvent Manager

Safety Summary
To protect yourself from harm and to prevent malfunctioning of the system, please observe
the following guidelines when operating the instrument:
Before using the instrument, pay attention to the warnings presented in the beginning
of the manual.
Wear the appropriate protective clothing, including safety glasses and gloves, when
preparing samples and solutions for use with this instrument.
Always follow the correct safety procedure and the manufacturer's recommendations
when using solvents.
Keep solvents with a boiling point less than 30 C under helium (10 kPa) in an optional
solvent cabinet.
Do not keep buffer solutions in the system when the instrument is not in use, since salt
may crystallize out.
Do not use acidic chlorides with pH less than 7; they can cause corrosion. Chloroform
and tetrachloromethane decompose slowly and form HCl.
Do not use chloride TRIZMA buffers since they form HCl in equilibrium. Use phosphate
buffers instead.
Do not use inorganic acids, concentrated organic acids or acidic buffer solutions.
Ensure that the system is flushed with degassed solvent.
Ensure that the other instruments in the system are ready to run.
Ensure that all connecting communications and power cables are correctly installed for
your analysis.
It is possible to clean the exterior surfaces of the instrument with a soft cloth dampened
with a mild detergent and water solution. Do not use abrasive cleaners or solvents.
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 warnings
used 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 and
instrument specifications.
Chapter 4 Installation
Information on installing and re-installing your instrument should you ever need to move
your system is provided.
Chapter 5 Maintenance
Maintenance and cleaning procedures for the various components of your instrument are
provided.
10 . Flexar Solvent Manager

Conventions Used in this Manual
Normal text is used to provide information and instructions.
Bold text refers to text that is displayed on the screen.
UPPERCASE text, for example ENTER or ALT, refers to keys on the PC keyboard. '+' is used
to show that you have to press two keys at the same time, for example, ALT+F.
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.
Notes, Cautions, and Warnings
Three terms, in the following standard formats, are also used to highlight special
circumstances and warnings.
NOTE: A note indicates additional, significant information that is provided with some procedures.



Introduction . 11


CAUTION


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

D
Caution (Achtung)
Bedeutet, da die genannte Anleitung genau befolgt werden mu, um
einen Gerteschaden zu vermeiden.
DK
Caution (Bemrk)
Dette betyder, at den nvnte vejledning skal overholdes nje for at
undg en beskadigelse af apparatet.
E
Caution (Advertencia)
Utilizamos el trmino CAUTION (ADVERTENCIA) para advertir sobre
situaciones que pueden provocar averas graves en este equipo o en
otros. En recuadros ste se proporciona informacin sobre este tipo de
circunstancias.
F
Caution (Attention)
Nous utilisons le terme CAUTION (ATTENTION) pour signaler les
situations susceptibles de provoquer de graves dtriorations de
l'instrument ou d'autre matriel. Les dtails sur ces circonstances
figurent dans un encadr semblable celui-ci.
I
Caution (Attenzione)
Con il termine CAUTION (ATTENZIONE) vengono segnalate situazioni
che potrebbero arrecare gravi danni allo strumento o ad altra
apparecchiatura. Troverete informazioni su tali circostanze in un riquadro
come questo.
NL
Caution (Opgelet)
Betekent dat de genoemde handleiding nauwkeurig moet worden
opgevolgd, om beschadiging van het instrument te voorkomen.
P
Caution (Ateno)
Significa que a instruo referida tem de ser respeitada para evitar a
danificao do aparelho.

12 . Flexar Solvent Manager





WARNING

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

D
Warning (Warnung)
Bedeutet, da es bei Nichtbeachten der genannten Anweisung zu
einer Verletzung des Benutzers kommen kann.
DK
Warning (Advarsel)
Betyder, at brugeren kan blive kvstet, hvis anvisningen ikke
overholdes.
E
Warning (Peligro)
Utilizamos el trmino WARNING (PELIGRO) para informarle sobre
situaciones que pueden provocar daos personales a usted o a
otras personas. En los recuadros como ste se proporciona
informacin sobre este tipo de circunstancias.
F
Warning (Danger)
Nous utilisons la formule WARNING (DANGER) pour avertir des
situations pouvant occasionner des dommages corporels
l'utilisateur ou d'autres personnes. Les dtails sur ces circonstances
sont donnes dans un encadr semblable celui-ci.
I
Warning (Pericolo)
Con il termine WARNING (PERICOLO) vengono segnalate situazioni
che potrebbero provocare incidenti alle persone. Troverete
informazioni su tali circostanze in un riquadro come questo.
NL
Warning (Waarschuwing)
Betekent dat, wanneer de genoemde aanwijzing niet in acht wordt
genomen, dit kan leiden tot verwondingen van de gebruiker.
P
Warning (Aviso)
Significa que a no observncia da instruo referida poder causar
um ferimento ao usurio.



Safety Practices
14 . Flexar Solvent Manager


Safety Practices . 15

Overview
This chapter describes the general safety practices and precautions that must be observed
when operating the Flexar Solvent Manager.
This advice is intended to supplement, not supersede, the normal safety codes in the user's
country. It is also a supplement to the PerkinElmer standard Safety and Health Policy. The
information provided does not cover every safety procedure that should be practiced.
Ultimately, maintenance of a safe laboratory environment is the responsibility of the analyst
and the analyst's organization.
Please consult all manuals supplied with the Flexar Solvent Manager and accessories before
you start working with the instrument. Carefully read the safety information in this chapter
and in the other manuals supplied. When setting up the instrument or performing analyses or
maintenance 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 the
voltage used in your laboratory.
Never remove the cover panels from the Flexar Solvent Manager without first shutting it
down and disconnecting the power cord from line power.
16 . Flexar Solvent Manager

General Operating Conditions
Only use the Flexar Solvent Manager indoors in a non-explosive environment and under the
following conditions:
Temperature 10
o
C to 35
o
C
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
o
C to 40
o
C
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

Safety Practices . 17

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, and
corrosive 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 except
as described in the accompanying User Documentation. Only a PerkinElmer service
representative or similarly trained and authorized person should be permitted to service
the instrument.
Whenever it is possible that the instrument is no longer electrically safe for use, make
the 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 under
unfavorable conditions; or has been subjected to severe stress during transportation.









18 . Flexar Solvent Manager

WEEE Instructions for PerkinElmer Products
or
A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that the
product is covered by the Waste Electrical and Electronic Equipment (WEEE) Directive and is
not to be disposed of as unsorted municipal waste. Any products marked with this symbol
must 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 the
environment, protect human health, and utilize natural resources prudently and rationally.
Specific treatment of WEEE is indispensable in order to avoid the dispersion of pollutants into
the recycled material or waste stream. Such treatment is the most effective means of
protecting the customers environment.
Requirements for waste collection, reuse, recycling, and recovery programs vary by
regulatory authority at your location. Contact your local responsible body (e.g., your
laboratory manager) or authorized representative for information regarding applicable
disposal regulations. Contact PerkinElmer at the web site listed below for information specific
to 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. These
other producers are directly responsible for the collection and processing of their own waste
products under the terms of the WEEE Directive. Please contact these producers directly
before discarding any of their products.
Consult the PerkinElmer web site (above) for producer names and web addresses.
Safety Practices . 19

Decontamination and Cleaning
Before using any cleaning or decontamination methods except those specified by
PerkinElmer, users should check with PerkinElmer that the proposed method will not damage
the equipment.
Decontamination
Customers wishing to return instrumentation and/or associated materials to
PerkinElmer for repair, maintenance, warranty or trade-in purposes are advised
that all returned goods must be certified as clean and free from contamination.
The customers responsible body is required to follow the "Equipment Decontamination
Procedure" and complete the Certificate of Decontamination. These documents are
available 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 Customer
Support.
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 PerkinElmer
sales office for more information.
Cleaning the Instrument
Exterior surfaces may be cleaned with a soft cloth, dampened with a mild detergent and
water solution. Do not use abrasive cleaners or solvents.

20 . Flexar Solvent Manager

ElectroMagnetic Compatibility (EMC)
Europe
All information concerning EMC standards is in the Declaration of Conformity, and these
standards may change as the European Union adds new requirements.
PerkinElmer instruments have been designed and manufactured, having regard to the state
of the art, to ensure that:
a. the electromagnetic disturbance generated does not exceed the level above which radio
and telecommunications equipment or other equipment cannot operate as intended;
b. it has a level of immunity to the electromagnetic disturbance to be expected in its
intended use which allows it to operate without unacceptable degradation of its intended
use.
Labels on Instrument






Safety Practices . 21

Quality Control/Good Laboratory Practices
The user should develop appropriate quality control procedures for the instrument to ensure
suitability for its intended use. These procedures typically consist of periodic performance
verifications and routine inspections and suitability tests.
Certificate of System Control
Each instrument is carefully built and tested in a controlled system in accordance with the
requirements specified in its applicable PerkinElmer Final Assembly and Test Specification.
Each instrument is certified to meet its functional and performance specification upon release
to 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 and
safe handling practices. Observe the manufacturers recommendations for use, storage and
disposal. 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 may
become hazardous after completion of an analysis. The responsible body
(e.g., Lab Manager) must take the necessary precautions to ensure that
the surrounding workplace and instrument operators are not exposed to
hazardous levels of toxic substances (chemical or biological) as defined
in the applicable Material Safety Data Sheets (MSDS) or OSHA, ACGIH,
or COSHH documents. Venting for fumes and disposal of waste must be
in accordance with all national, state and local health and safety
regulations and laws.
Definitions in Warning for Hazardous Chemicals
Responsible body: Individual or group responsible for the use and maintenance of
equipment, and for ensuring that operators are adequately
trained. [per IEC 61010-1]
Operator: Person operating equipment for its intended purpose. [per IEC
61010-1, ]
OSHA: Occupational Safety and Health Administration (United States)
ACGIH: American Conference of Governmental Industrial Hygienists
COSHH: Control of Substances Hazardous to Health (United Kingdom)


22 . Flexar Solvent Manager

Safe Handling of Solvents

WARNING
Give careful attention to the hazards associated with the
solvents you are using. Refer to the safety data sheets
provided by the manufacturer. For example, Material Safety
Data Sheets (MSDS) in the USA.



WARNING
Do not use the Solvent Manager to degas perfluorinated
solvents. Teflon AF is soluble in solvents such as the
Fluorinert series from 3M company and PF series from
Ausimont. Where there is a question about using a particular
solvent that is fluorinated, contact a PerkinElmer
representative.

Wear appropriate eye protection at all times when handling chemicals. Use safety
glasses with side shields, goggles, or full-face shields, according to the types of
chemicals you will be handling.
Wear suitable protective clothing, including gloves that are specifically resistant to the
chemicals being handled.
Always use clean solvents. Solvents which have been distilled in glass (HPLC Grade) are
recommended.
Filter the solvents and buffers through a 0.5-micron medium as an additional
precaution.
Degas all aqueous and most organic solvents prior to use.
Store flammable solvents or solvents which may form hazardous by-products when the
instrument 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.

Safety Practices . 23

Buffers
Exercise care when using buffers in conjunction with organic solvents. NEVER LEAVE
BUFFERS IN THE SYSTEM OVERNIGHT. Buffers left in the system can form salt crystals
which may cause premature injector valve failure and plug the transfer tubing and sample
needle. 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 using
buffers.
Corrosion
The following corrosion precautions apply to the standard (stainless steel) and the
biocompatible (titanium) instruments.
All parts of the instrument that contact mobile phase are made of stainless steel, KelF, and
quartz. Some of these materials are extremely sensitive to acid chlorides. If you have
questions 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 Chloride
Dichloromethane
Sulfuric Acid (Conc.)
Hydrochloric Acid (20% and 37%)
Hydrofluoric Acid (20%, 50%, and 75%)
Copper Chloride
Bromine
Freon 12 (wet)
Chlorinated solvents
Hydrofluorosilicic Acid (20%)
Hydrobromic Acid (20%)
Ferric Chloride
Ferrous Chloride
Mercuric Chloride (Dilute)
If you have questions about your mobile phase, contact a PerkinElmer representative. Refer
to 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 a
heated 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.
24 . Flexar Solvent Manager

Auto-Ignition Temperatures of Common LC Solvents.

Solvent
Auto-Ignition
Temperature (C)
Carbon Disulfide 100
Diethyl Ether 180
Cyclohexane 260
Hexane 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 not
occur, observe the following precautions:
Ensure that the pump's solvent inlet filter is below the solvent level in the solvent
reservoir.
If the pump has not been used for an extended period of time, remove air bubbles by
connecting 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 the
drain valve completely.
If bubbles are observed in the flow cell, degas the solvent and add back-pressure device
P/N 09907126.




Description






Description . 27

Overview
The Solvent Manager is a high-efficiency in-line module that removes dissolved gasses from
HPLC solvents. Its unique design assures reliable continuous operation and the highest level
of continuous performance available without the need for helium degassing. Up to five
solvent lines may be degassed simultaneously by one unit. The extremely low internal
volume of each Teflon AF

channel offers very quick equilibration and very short startup


times 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 is
located in a vacuum chamber. Within this chamber a partial vacuum is maintained by a
constantly running, low RPM vacuum pump. Dissolved gasses migrate across the tubing wall
under 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 vacuum
level by varying the vacuum pump speed as needed.
A special port in the vacuum pump continually flushes the pump head with a small bleed of
air to remove any solvent vapors which may enter the pump from the vacuum chamber. This
air bleed eliminates the need for any solenoid valves within the system. This patented*
design results in zero vacuum hysteresis. Previous designs allowed the vacuum chamber
pressure 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 vacuum
sensor signal to confirm that it is within an expected range. Following the startup test, the
microprocessor ramps the vacuum pump to high RPM, to quickly exhaust atmosphere from
the vacuum chamber. As the vacuum level approaches the preset control value, the pump
RPM will slowly ramp down to a low speed (typically 40 to 60 RPM). Afterwards, the pump
RPM will vary slightly, as needed under the changing degassing load, to maintain a virtually
constant 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

degassing
tubing. Only a ZHCR

design ensures a baseline which is unaffected by the degasser.



28 . Flexar Solvent Manager

Solvent Manager Status LEDs
The Flexar Solvent Manager status is displayed on the front panel through the following
indicator lights.





LED Functionality

Power On LED Instrument Status
OFF 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 On
LED
Ready/Error
LED
Vacuum
LED
Green Green/Red Green/Red
Description . 29

Principles of Operation
The Flexar Solvent Manager vacuum degasser consists of a vacuum chamber, degassing
tube, variable speed vacuum pump, microprocessor controller, sensor, and check valves. The
solvent (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 the
mobile phase across the tube wall, in accordance to Henrys Law, thus degassing the mobile
phase. The pressure in the vacuum chamber is established by the vacuum pump and
monitored by the microprocessor through an integrated absolute pressure sensor. Degassed
mobile 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 the
vacuum degassing system can be observed by monitoring the RPM of the pump. This smart
leak detection is a benefit of the patented design of the degasser. If a leak occurs within
the chamber, the microprocessor will increase the pump RPM in an attempt to maintain the
vacuum level. If the pump cannot maintain the vacuum level (if it runs at an elevated RPM
for more than 2 minutes), the red LED will flash, indicating a possible leak condition, and the
system 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 other
fluoropolymers. The fully amorphous nature of this fluoropolymer and its molecular structure
creates a molecular level porosity unlike the mechanically induced porosity in PTFE extruded
tubing. In addition, unlike the process used in extruding PTFE, no extrusion agents are
needed (like kerosene, etc.) which contaminate mobile phases until they are extracted by the
mobile phase over time. Likewise, this molecular structure, combined with the very small
surface areas required to degas the mobile phase, reduces the possibility of carryover from
one solvent or mobile phase to another to virtually zero.
30 . Flexar Solvent Manager

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, and
when combined with the ultra-low internal volumes of Teflon AF

channels needed for HPLC


flow 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 years
without concern for normal HPLC solvents. However, Teflon AF

is soluble in certain
solvents (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 the
vacuum pump in the vacuum degasser contains internal provisions for sweeping water or
solvent vapor from the pump continuously, it is possible that over time, high concentration
buffers may form crystals within the channel due to the loss of water within the channel. The
same precautions should be taken to prevent crystallization within these channels as are
taken 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 version
Degassing Process Gas permeation through a fluoropolymer membrane
Maximum Recommended Flow
Rate
1

3.0 mL/min.
Pressure Drop
2
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 channel
Materials contacting solvents PEEK, Glass-filled PTFE, Teflon AF


Power:
Power requirement 100 to 240 VAC (10%), 1A, 47 to 63 Hz
Power Supply Adapter Plugs 4 supplied with power supply, interchangeable: North
America/Japan, U.K., Continental Europe, Australia
Installation 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 C
Ambient Relative Humidity (RH) 20 to 80 % RH (without condensation)
Altitude 0 to 2000 Meters
Indoor vs. Outdoor Use Indoor
Pollution Degree 2
Storage Conditions:
Ambient temperature -20 to +60 C
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 estimate
assumes low pressure mixing and low flow restriction prior to the HPLC pump. MeOH/Water mixing represents
the worst outgassing case and maximum flow rate will likely increase with Acetonitrile/Water mixtures. High
pressure 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 and
outlet bulkheads may contribute to the overall pressure, but are not included in the estimate.


32 . Flexar Solvent Manager









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 the
detector performance should be considered hazardous to
someone 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 other
instruments 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 required
for performance verification.
Waste-Solvent Disposal
Provide a properly labeled chemical waste container in a safe and vented place. Make sure that it is
within all of the specified safety requirements for your location. Wear gloves, eye protection, and a
laboratory coat when handling or disposing of chemical waste.
Electrical Requirements
The AC power supply supplied with the vacuum degasser incorporates a universal AC input, switching
regulator. 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 and
automatically adjusts its operation accordingly. The switching regulator assembly incorporates its own
on-board line voltage fuse. This fuse is not user serviceable. In the event that this fuse blows, it will be
necessary 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 the
standard 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.
36 . Flexar Solvent Manager

Unpacking

CAUTION
Take great care when installing your Solvent Manager, and
follow the procedures described in this manual. If you require
assistance, contact your local PerkinElmer Service Engineer.
Carefully unpack the Flexar Solvent Manager and check for obvious signs of damage that may have
occurred during shipment. Immediately report any damaged or missing items to the shipping carrier and
PerkinElmer.
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)
Users Guide on CD 1
Port Plug, -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 be
positioned 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-channel
vacuum degasser and other instruments in an LC system. The direction of flow through the vacuum
degasser 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
HPLC
Pump
Autosampler
Wash
Auto-
Sampler
Solvent Manager
A
B
C
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 m filter frits.
The Flexar Solvent Manager with 5-CH vacuum degassing includes two 2L , two 1L, and one
500mL bottles, fitted with caps, tubing and 10 m 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) connect
tubing from each bottle to channel A and B on the top row of the solvent connectors to each
38 . Flexar Solvent Manager

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

5. Connect the tubing from each channel (A, B, C) on the bottom row to the corresponding pump
inlets. 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. The
upper 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 the
vacuum degasser.
2. Push the tubing through a PEEK 1/8 male -28 fitting and slide a ferrule over the tubing end (see
figure below). Cut the Teflon tubing so the end is flat.
3. Screw the -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 be
tightened 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 unused
ports 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 and
drawing air and/or mobile phase into the syringe until no air remains in the tubing, approximately
5 milliliters.
Installation . 39


CAUTION
DO NOT prime the membranes by pushing solvent through the
degassing systems. This technique can generate several hundred
pounds of pressure which might rupture the membrane, even though
the Teflon AF

membrane is quite rugged. The maximum


recommended 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 to
the 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 that
plugs are installed in the unused ports.
4. Disconnect and remove the tubing that is connected to the output port (the lower row of
connectors), connect the priming syringe to this port, and pull the solvent through the degasser
until 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 -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 until
you achieve leak-free operation.
The vacuum degasser maintains a constant vacuum pressure of 50 mm Hg absolute (nominal) by
varying 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 and
pump speed is constantly monitored by the microprocessor for changes in operating conditions
which might be attributed to chamber internal leaks. If a potential leak is detected, the pump will
be 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 degassed
so 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 power
connector on the rear of the vacuum degasser and start the pump at 1.0 mL/min.
40 . Flexar Solvent Manager


Allow the system to equilibrate for 5-10 minutes. The small volumes contained in the Flexar Solvent
Manager vacuum degasser should only be considered in chromatograph equilibration time when
flow rates less than 1 mL/min are used.
Immediately upon turning on the vacuum degasser, the microprocessor examines the vacuum
sensor signal to confirm that it is within an expected range. Following the startup test, the
microprocessor ramps the vacuum pump to high RPM, to quickly exhaust atmosphere from the
vacuum chamber. As the vacuum level approaches the preset control value, the pump RPM will
slowly ramp down to a low speed (typically 40 to 60 RPM) and will vary slightly as needed under the
changing 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 is
running, beyond the front panel LEDs, the slight vibration caused by the microstepping of the motor
driving 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 connected
is 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 solvent
vapors 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 of
solvent (approximately 480 microliters). When changing from one solvent to another where the final
solvent is immiscible with the first, use an intermediate solvent miscible with both the initial and final
solvent. 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 solvent
reservoir 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 pump
to draw each solvent to be used in the analysis at a flow rate of 2 mL/min. for 1-2 minutes. This ensures
that the line from the degasser channel being primed through the proportioning valve on the pump has
freshly degassed solvent. This dynamic priming method will allow an immediate startup of the analysis
upon 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, PTFE
channels 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 not
properly degassed. These solvents are generally alcohols (e.g. methanol), acetonitrile and
tetrahydrofuran. 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 is
generated by your vacuum degasser or pump at a flow rate of 3 mL/min. If outgassing does occur, or if
a flow rate higher than 3 mL/min. is required, it is a general rule that only the organic portion of the
mobile phase needs to be passed through a second degassing channel to ensure outgassing does not
occur. This is due to the ability of all organic solvents (e.g. methanol) to hold at least 10 times more
dissolved atmosphere than water can.
To more thoroughly degas a mobile phase, connect the outlet of the organic channel to the inlet a
second channel and the outlet of the second channel to the pump. This places the two channels in series
and 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 harmful
deposits 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 the
system with water. Evaporation leaves salt crystals that may form harmful deposits. Remove
chloroform 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 excluded
from warranty.
3. After removing harmful mobile phases, prepare the detector for most mobile phases by flushing it
with 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 off
the 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 degasser
first with water and then with isopropanol.
42 . Flexar Solvent Manager

3. Turn off the vacuum degasser. Then disconnect the tubing between the vacuum degasser and
solvent reservoirs and the vacuum degasser and pump. Plug all of the ports on the vacuum
degasser.
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 column
before reconnecting the column and restarting the system.





Maintenance

44



Maintenance . 45

Preventive Maintenance
Preventive maintenance ensures that your Solvent Manager will perform consistently at an
optimal 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 detector
connections. (The tubing available from PerkinElmer is passivated.)
Follow the short- and long-term shutdown procedures.
46 . Flexar Solvent Manager

Troubleshooting Guide
Problem Probable Cause Solution
1) The AC power is plugged in but
all 3 LEDs are off, indicating no
power 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 seems
high.
2) Pump is in initial pull-down
phase or systems degassing
demand has increased.
2) Typically normal operation,
although if pump speed continues
to rise for an extended period of
time (as heard by the pitch of the
stepper motor) it could indicate a
potential fault condition.
3) Status LED is flashing
approximately 1 second off, 1
second on. Vacuum pump is not
running.
3) Possible system leak. 3) Contact your Service
Representative.
4) Status LED is flashing
approximately 2 seconds off, 1
second on. Vacuum pump is not
running.
4) Possible sensor or Control
Board fault.
4) Contact your Service
Representative.

5) Is there a way to check
whether the system is operating
correctly when Power and
Vacuum green LEDs are
illuminated, but pump cant be
heard running?
5) Due to the design of the pump
and degasser, the pump is
virtually silent at low RPM, even
though vacuum is good and
degassing is normal.
5a) Place a hand on the top of the
unit. A slight vibration can be felt
indicating the pump is operating
at low RPM.
5b) Monitor the UV absorbance of
non-degassed methanol at 215
nM versus degassed methanol
coming through the degasser.
Proper performance of the
degasser should decrease the UV
absorbance of the methanol
significantly.
6) Bubbles appear through the
output tubing.
6) Loose fitting(s). 6) Tighten the input and output
fittings.
7) No solvent flow. 7a) Air in the HPLC pump head.
7b) If a buffer solvent was left in
the degasser for some time after
use, it may plug the degasser
elements.
7a) Prime/purge the pump head.
7b) Use a different channel, or
connect the channel to a beaker
of the solvent without the buffer.
Draw the solvent through the
channel to dissolve the buffer.
Do not push the solvent through
the channel. If this flushing
action does not work, contact
your Service Representative.


Maintenance . 47

Index
A
About This Manual ................................................ 9
Air Bubbles..........................................................24
B
Bench Space, providing adequate .........................35
Buffers................................................................23
C
Chemicals
Definitions of Warnings ...................................21
Hazardous ......................................................21
Cleaning the Instrument.......................................19
Conventions
Notes, cautions and warnings ..........................10
text ................................................................10
Corrosion ............................................................23
D
Decontamination .................................................19
Degasser Operation .............................................27
Degasser Performance .........................................30
Degasser Schematics ...........................................29
Degassing flow rate range....................................40
E
Electrical Safety...................................................17
ElectroMagnetic Compatibility ...............................20
Environmental Conditions.....................................16
H
HPLC grade solvents ............................................35
I
Installation
start-up kit......................................................36
Instrument Specifications .....................................31
L
Laboratory Practices
GLP ............................................................... 21
O
Operating summary............................................. 39
P
Precautions......................................................... 15
Preventive Maintenance....................................... 45
Principles of Operation ........................................ 29
Q
Quality Control .................................................... 21
S
Safety
Summary ......................................................... 8
Safety Information .............................................. 15
electrical safety .............................................. 17
environmental conditions ................................ 16
Shutdown........................................................... 41
long-term....................................................... 41
short-term ..................................................... 41
Solvents ............................................................. 22
Auto-Ignition Temperature.............................. 23
Low boiling points .......................................... 22
Specifications...................................................... 31
Start-up Kit......................................................... 36
Storage Conditions.............................................. 16
System Description
major components.......................................... 28
specifications.................................................. 31
T
Teflon-AF Membranes ......................................... 29
Troubleshooting Guide ........................................ 46
W
Warnings
Hazardous Chemical ....................................... 21
Waste and Solvent Disposal ................................. 35
WEEE Instructions............................................... 18

Você também pode gostar