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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
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All rights are reserved. No part of this publication may be reproduced in any form whatsoever or
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Registered names, trademarks, etc. used in this document, even when not specifically marked as such,
are protected by law.
Table of Contents
Tube management clips are integrated into all four corners of the detector front fascia assure
secure tubing positioning while allowing flexibility in tubing configuration. Integrated drain
tray and inter-component drain management are also built into front fascia to provide
protection against leaks (the drain management is designed for plug-and-lay with all other
Flexar components).
A color-coded front panel LED display indicates power, system status, and detector lamp
status. An easily-removable magnetized front panel provides immediate access to the
detector.
The detector includes stand-alone calibration and maintenance software package. It also can
be controlled by the TotalChrom Chromatography (WS/CS) Data Systems with the associated
LC IPM. The PDA requires but does not include the dotLINK box for use with TotalChrom. It
also requires but does not include IRIS™ Spectral Processing software for access / display of
spectral data.
This manual contains important information regarding potential hazards that may arise
during the operation of the Flexar PDA Detector. It is essential that the Safety and
Regulatory information preceding this chapter be read and thoroughly understood by all
users and potential users of the detector.
This manual was written for a person who has developed a working knowledge of liquid
chromatography and understands:
• the function of each major component in a liquid chromatography system
• how to select a column based on the analysis that will be performed
• the principles of solvent selection and sample preparation
If you require an introduction to these concepts, the following book is an excellent reference:
Practical Liquid Chromatography -- An Introduction by R.W. Yost, L.S. Ettre, and R.D. Conlon,
published by PerkinElmer (1980), P/N 09939656.
8 . Flexar PDA LC Detector
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
Chapter 1 Introduction
This chapter contains a brief introduction on the instrument, the conventions and warnings
used in the manual.
The preparation of your laboratory needed for the Flexar PDA Detector. Laboratory
requirements for the instrument are reviewed in this chapter.
Chapter 4 Description
This chapter contains information on the components of the instrument, how it works and
instrument specifications.
Chapter 5 Installation
Information on installing and re-installing your instrument should you ever need to move
your system is provided.
Chapter 6 Maintenance
Maintenance and cleaning procedures for the various components of your instrument are
provided.
10 . Flexar PDA LC Detector
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.
NOTE: A note indicates additional, significant information that is provided with some procedures.
Introduction . 11
We use the term CAUTION to inform you about situations that could
CAUTION
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, daß die genannte Anleitung genau befolgt werden muß, um
einen Geräteschaden zu vermeiden.
DK Caution (Bemærk)
Dette betyder, at den nævnte vejledning skal overholdes nøje for at
undgå en beskadigelse af apparatet.
E Caution (Advertencia)
Utilizamos el término CAUTION (ADVERTENCIA) para advertir sobre
situaciones que pueden provocar averías graves en este equipo o en
otros. En recuadros éste se proporciona información sobre este tipo de
circunstancias.
F Caution (Attention)
Nous utilisons le terme CAUTION (ATTENTION) pour signaler les
situations susceptibles de provoquer de graves détériorations de
l'instrument ou d'autre matériel. Les détails sur ces circonstances
figurent dans un encadré semblable à 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 (Atenção)
Significa que a instrução referida tem de ser respeitada para evitar a
danificação do aparelho.
12 . Flexar PDA LC Detector
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.
WARNING
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 ikke
overholdes.
E Warning (Peligro)
Utilizamos el término WARNING (PELIGRO) para informarle sobre
situaciones que pueden provocar daños personales a usted o a
otras personas. En los recuadros como éste se proporciona
información sobre este tipo de circunstancias.
F Warning (Danger)
Nous utilisons la formule WARNING (DANGER) pour avertir des
situations pouvant occasionner des dommages corporels à
l'utilisateur ou à d'autres personnes. Les détails sur ces circonstances
sont données dans un encadré semblable à 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 não observância da instrução referida poderá causar
um ferimento ao usuário.
Introduction . 13
Overview
This chapter describes the general safety practices and precautions that must be observed
when operating the Flexar PDA Detector.
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 PDA Detector 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
The following precautions must be observed when using the Flexar PDA Detector:
• Be sure that the voltage of the Flexar PDA Detector corresponds to the voltage used in
your laboratory.
• Never remove the side panels of the Flexar PDA Detector without shutting down the
instrument and disconnecting the instrument power cord from line power.
18 . Flexar PDA LC Detector
Temperature 10 oC to 35 oC
Altitude up to 2000 m
Avoid any adjustment, maintenance and repair of the opened, operating instrument. If any
adjustment, maintenance and repair of the opened instrument is necessary, this must be
done by a PerkinElmer Service engineer or a similarly trained and authorized person.
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
• Pollution degree 2
Storage Conditions
The instrument may be stored under the following conditions:
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. The supply must
have a correctly installed protective conductor (earth ground) and must be installed or
checked by a qualified electrician before connecting the instrument.
• Always turn off the all components to the detector and disconnect the power cord from
the electrical outlet before you remove any covers. Do not operate the instrument with
any covers or internal parts removed.
• Disconnect the instrument from all voltage sources before opening it for any
adjustment, replacement, maintenance, or repair. If afterwards, the opened instrument
must be operated for further adjustment, maintenance, or repair, this must only be
done by a PerkinElmer Service engineer a similarly trained and authorized person. Use
only fuses of the specified type and with the required current rating for replacement.
• 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.
• 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.
20 . Flexar PDA LC Detector
• Be sure the power cord is the correct one for your laboratory. The line cord used must
meet the national safety agency’s guidelines for the particular country of use. Some
power cords available from PerkinElmer are illustrated below:
Europe Australia
Switzerland ETSA S/86
09991413 09991417
Europe Israel
Italy 09991424
09991422
Denmark Japan
09991416 09991425
China
09290348
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 customer’s 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.
22 . Flexar PDA LC Detector
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.
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.
If you are located outside of the United States or Canada, please call your local PerkinElmer
sales office for more information.
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.
24 . Flexar PDA LC Detector
Labels on Instruments
Warning
Disconnect supply cord before opening.
Grounding circuit contin uity is vital for Warning
safe operation of equipment. Never For prote ction against fire hazard,
operate equipment with grounding replace only with same type and
conduct or disconnected. rating of fuse.
Warning
Warning
ETHERNET
VIS
COM 1
100 -240 - VAC
50/60 Hz, 195VA
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.
While the Universal Test Mix (UTM) P/N 00890893 can be used for a system check, we
recommend that you develop a separate system suitability test and acceptance criteria for
each of your assays.
Hazardous Chemicals
Before using mobile phase solvents, you should be thoroughly familiar with all hazards and
safe handling practices. Observe the manufacturer’s recommendations for use, storage and
disposal. These recommendations are normally provided in the material safety data sheets
(MSDS) supplied with the solvents.
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, ]
• 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.
• Store flammable solvents or solvents which may form hazardous by-products when the
instrument is shut down, by following the recommended shutdown procedure.
• Know the relative polarity and miscibility of the solvents being used.
WARNING
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.
28 . Flexar PDA LC Detector
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.
If you have questions about your mobile phase, contact a PerkinElmer representative. Refer
to the table below:
WARNING
WARNING
Safety Practices . 29
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.
Pressure Buildup
Over time, you may observe a gradual increase in the system operating pressure. If you
observe pressure readings greater than 3.45 MPa (500 psi) above the normal operating
pressure of your analysis, the following items may need attention:
30 . Flexar PDA LC Detector
• If you are injecting “clean” samples and there is no other apparent cause for the
pressure build-up, remove, disassemble, and clean the flow cell.
• If you are injecting “dirty” samples, the flow cell may be clogged or the column packing
material may have retained contaminated particulates. Remove and clean the flow cell,
and replace the column.
• The column end fitting or column frit may be plugged. Replace the end fitting or frit to
relieve excess pressure.
Fuses
Overview
Before installing your Flexar PDA Detector, prepare your laboratory according to the following
guidelines:
Environmental Conditions
The laboratory in which the Flexar PDA Detector is located must meet the following
conditions:
• A corrosive-free environment.
• The instrument will operate with a laboratory temperature between 10 and 35 °C (50 °F
and 95 °F).
• Constant relative humidity between 20% and 80% (without condensation)
The Flexar PDA Detector has been designed for indoor use. Do not use the instrument in an
area where explosion hazards may exist.
flammable caustic
explosive corrosive
toxic
Use care when working with hazardous solvents, or solvents that produce hazardous by-
products.
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.
WARNING
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 Flexar PDA Detector requires a grounded nominal 100 – 240 VAC source. The detector
uses 195 VA maximum power. Data processing equipment and other accessories require
separate outlets. (Refer to the appropriate instrument manual for the power requirements.)
To prevent degradation of the detector’s performance, the AC line voltage must remain
within + 6% / -10%of the specified voltage range. If there are large voltage fluctuations,
install a voltage regulator between the detector and the AC outlet.
WARNING
Description
36 . Flexar PDA LC Detector
Description . 37
The Power On/Off Switch on the LED panel is used with the Main Power Switch on the
rear panel. You must first switch on the Main Power Switch on the rear panel then push and
hold the Power On/Off Switch on the LED panel until you see the power on LED turn green.
LED Functionality
Power On LED Instrument Status
OFF OFF
OFF Standby
ON (green) ON
• COM 1 – Connects to the dotLINK Port F to communicate via the RS232 cable
• CONTROL – Connects to the dotLINK Port B to receive commands from the dotLINK to
initiate runs.
COM 1
100 -240 - VAC
50/60 Hz, 195VA Fuse Holder
Figure 3 Connectors at the rear of the Photo Diode Array (PDA) Detector
Description . 39
Operating Summary
Make sure that the PDA AC line cord is connected to the proper line voltage. See the
paragraphs "Electrical Requirements".
You control your Flexar PDA Detector through the TotalChrom software.
¾ TotalChrom users should install the Software on the CD to control your detector through
TotalChrom.
¾ Install the IRIS Spectral Processing Software to view and process data.
40 . Flexar PDA LC Detector
Specifications
Installation Summary
The installation of your detector is divided into the following steps:
• Tubing connections
• Instrument Start-up
NOTE: After completing the installation of the Flexar PDA Detector, carefully read TotalChrom
Connections and Methods before powering-up the detector.
Unpacking
Take great care when installing your Flexar PDA Detector, and
follow the procedures described in this manual. If you require
CAUTION assistance, contact your local PerkinElmer Service Engineer.
Carefully unpack the Flexar PDA Detector and check for obvious signs of damage that could
have occurred during shipment. Immediately report any damage or missing items to the
shipping carrier and PerkinElmer.
Items Included
A Start-Up Kit (P/N N2920612) for the Flexar PDA Detector is supplied with the detector. It
contains a CD containing the user’s guide and software utilities, cables, tubing, and other
items that are necessary to install your detector. You can order replacement parts from
PerkinElmer’s catalog service as described on the Customer Service page of this manual.
44 . Flexar PDA LC Detector
The Flexar PDA Detector can operate at 50 or 60 Hz and requires a grounded outlet that
provides a nominal 100, 120, 220, or 230/240 VAC source. If the electrical supply voltage in
your laboratory produces large AC line voltage fluctuations, install a voltage regulator
between the AC line voltage outlet and the Flexar PDA Detector. Instrument grounding is
required, and is accomplished by a third wire in the AC line-voltage outlet box. If your
electrical outlet does not contain a ground, contact your local electric company.
Fuse
Single Fuse
North American
Power Input
Module
Fuse
Dual Fuses
European Fusing
Figure 4 Fuses
1. Make sure the main power switch is in the OFF position. Remove the power cord from
the module.
2. Remove the power input module cover by inserting a small flat blade screwdriver into
the notch and gently pry it up until you see the door separate from the module.
4. Gently pry the fuse holder out of the power input module.
5. Insert the fuse that corresponds to your location into the fuse holder.
One side accepts a single fuse and the other side accepts dual fuses. Use only 2.5-amp T
type fuses (P/N 09991650).
Installation . 45
6. Insert the side of the fuse holder containing the fuse(s) for your location as you align
the slot in the fuse holder with the pin in the power input module.
WARNING
The line cord should have the electrical rating and plug
appropriate for your location. See the figure below for the
correct cord.
2. Insure that the power switch is off and insert the line cord plug into the AC supply.
Europe Australia
Switzerland ETSA S/86
09991413 09991417
Europe Israel
Italy 09991424
09991422
Denmark Japan
09991416 09991425
China
09290348
Tubing Connections
The flow cell is shipped with 0.007 in. ID standard stainless steel tubing installed. Make all
connections with standard 1/16-in. fingertight fittings.
46 . Flexar PDA LC Detector
• Client/Server installation requires a client PC with acquire capability and IRIS Spectral
Processing Software
• Workstation installation requires only TotalChrom Workstation software and IRIS
Spectral Processing Software
Hardware/Software Requirements
The following are the software requirements for using the Flexar PDA Detector with TotalChrom:
• TotalChrom WS/CS (6.3.1 or higher)
• IRIS Spectral Processing Software
• dotLINK interface
PORT DEVICE
Port (INST) A Pump
Port (INST) B PDA
Port (INST) C Autosampler
Port (INST) D none
Warning
Warning
ETHERNET
To Network VIS
or PC (TotalChrom)
COM 1 1 00 -240 - VAC
50/60 H z, 195VA
Use a Crossover type
cable if connecting
directly to a PC
CONTROL SPECTRAL DATA
P/N 09290144
P/N 09290144
dotLINK
P/N N2936018
P/N 09290148
Serial (RS232)
Communication
Flexar Pump
Flexar Autosampler
Figure 7 TotalChrom Connections
Setting up an LC Method
In the following paragraphs the autosampler, pump, and diode array detector parameters are
selected for the collection of chromatographic and spectral data. To use specific values for the
parameters, we set up the conditions for the analysis of the Universal Test Mix (P/N 00890893).
NOTE: For configuration information and procedures for building a method, refer to Chapters 3 and
5, respectively, of the TotalChrom Workstation User’s Guide (P/N N5156023 and N5156024).
From the TotalChrom Navigator screen, select Method Editor and create a new method by
selecting from the parameters and timed events listed below.
48 . Flexar PDA LC Detector
2. If you are using manual injection, select Manual. If you are using an autosampler, select
Autosampler and continue with Steps 3 through 20.
3. In the Injection Volume text box, enter the amount of sample that you want to inject.
(Make certain that this value is less than 50% of the Loop Size that you specify in step 4.)
4. From the Loop Size list, select the size of the injection loop fitted to your autosampler.
NOTE: To enable the Fixed Mode option, where the injection volume is equal to the loop volume,
select a loop size value less than 50 μL.
5. To operate in Fixed Mode, set the value of the Fixed Mode list to On. This option forces
the Injection volume to be equal to the loop volume. Fixed mode is useful if you are
working with small sample sizes or applications that require high precision. (You can
only use Fixed Mode when the Loop Size value is less than 50 µL.)
6. In the Excess Volume text box, enter the amount of sample that you want withdrawn
from the vial in addition to the injection volume.
(This option prevents evaporation and contamination by isolating the actual plug of
sample to be injected as it is transported to the injection loop. This option is only
available if Fixed Mode is set to Off.)
7. In the Air Cushion text box, enter the amount of air that you want to insert between the
sample and flush solutions to prevent the two solutions from mixing.
9. From the Sample Speed list, select the speed at which you want the sample pump to fill
the injection loop.
Installation . 49
(Slower speeds provide more reproducible injection volumes, particularly for viscous
samples.)
11. In the Inject Delay Time text box, enter the number of minutes that you want between
the pump's run start signal and when the sample injection occurs.
12. If you are using a Series 200 Autosampler, refer to “Creating Derivatization and Dilution
Programs.”
13. In the Flush Volume text box, enter the amount of flush solution that you want pumped
through the sampling system for each flush cycle.
14. From the Flush Speed list, select the speed at which you want the pump to flush the
system.
15. In the Flush Cycles text box, enter the number of flush cycles that you want to have
between injections when the method changes in a sequence.
(This value also specifies the number of flushes the autosampler performs when you
choose Flush Autosampler in the Hands On dialog box.)
16. In the Pre-Injection Cycles text box, enter the number of flush cycles that you want
before each sample injection or before each vial-to-vial transfer in sample processing
modes.
17. In the Post-Injection Cycles text box, enter the number of flush cycles that you want
after each sample injection or before each vial-to-vial transfer in sample processing
modes.
18. In the Post-Method Cycles text box, enter the number of flush cycles that you want
after each method is completed in a sequence.
19. Under Peltier Tray Control, set the temperature of the tray.
20. In the ± list, select a tolerance percentage to control when the system Peltier Tray
becomes ready.
(The Peltier Tray will be ready to inject only if the temperature is within the range of
the temperatures that you set, plus or minus the value in the tolerance section.)
50 . Flexar PDA LC Detector
1. Select the Pump Config tab of the Instrument Control dialog box.
2. In the Ready Time text box, enter the number of minutes that the pump remains in a
READY state, after which you want the pump to shut down. (A Ready Time of 999
means that the pump will continue in the READY state indefinitely.)
3. In the Standby Time text box, enter the number of minutes that the pump remains in a
READY state, after which you want the pump to change to the standby flow rate. (A
Ready Time of 999 means that the pump will continue to use the flow rate set in the
grid as long as the pump remains READY.)
4. In the Standby Flow text box, enter the pump flow rate for the standby mode.
5. From the Pressure Units list, select either PSI or BAR as the units for inlet pressure; the
choice depends on the instrument that you are using.
6. In the Max Pressure text box, enter the upper pressure limit, above which the pump will
shut off.
7. In the Min Pressure text box, enter the lower pressure limit, below which the pump will
shut off.
8. In the Solvent Names text boxes, enter the labels you want to use.
Installation . 51
You can enter 10 rows, or steps, in the pump program. Step 0 is always the pre-run
equilibration, for which you enter Time, Flow, and Solvent values. The table for Flexar LC
Pumps has the following columns:
• D (Solvent)−The percentage of this solvent at the end of each program step. This
value adjusts automatically so that the sum of A, B, C, and D is 100.
• Curve−type of gradient curve to use for this program step. The types of curve are step
(0), linear (1), convex (-1.1 to -9.9), and concave (1.1 to 9.9) for increasing solvent
percentage. The magnitude of the number determines the degree of curvature.
52 . Flexar PDA LC Detector
1. Select the Pump Program tab of the Instrument Control dialog box.
NOTE: The Program Time field displays the sum of the values in the Time column for all the steps
that you create. The Detector Time field displays the data acquisition time of the analysis
2. In Step 0 of the table, click in the Time, Flow, and solvent fields, and then enter
amounts for the equilibration step.
3. Enter the Time, Flow rate, solvent composition, and Curve type for each additional
program step.
4. The Time field activates the other fields in each row, and the curve changes as you
enter each set of values. Depending on the specific pump that you are using,
TotalChrom completes the solvent percentage either for solvent B or for solvent D so
that the total solvent composition is 100 percent. Also, if you change the value of
solvent B or the value of solvent D, the value of solvent A adjusts so that the total
remains 100 percent.)
NOTE: For the 250 pump, the resolution at which you can enter time and flow values, changes
across the allowed range. You can enter times between 0 and 9.9 minutes to the nearest 0.1
minute, but times between 10 and 999 minutes must be to the nearest minute. Flow rates
between 0 and 0.99 mL/min can be to the nearest 0.01 mL/min, but flows between 1.0 and
10.0 mL/min can only be to the nearest 0.1 mL/min. TotalChrom will beep if your entry
causes a change from one resolution range to another.
5. To reduce the amount of equilibration time after the first run, select Enable Solvent
Saver, and then enter the new amount of equilibration time to use after the first run in
the text box.
6. To turn the pump off at the end of the run without recycling to initial conditions, select
Shutdown in Final Conditions.
NOTE: Only set this option for a “shutdown method,” which is run as the last cycle in a sequence.
Installation . 53
LC Detector Parameters
The Detectors tab of the Instrument Control dialog box is used to set detector parameters:
• Bandwidth BW-A and BW-B − The bandwidth, or total wavelength range, around the
nominal selected wavelength for Channels A and B.
• Spectral Acquisition parameters − which can be Off and Time. If Time is selected, you
will select the rate at which spectra will be selected.
1. Enter 254 (nm) for the Channel A Wavelength and 280 (nm) for the Channel B
wavelength.
3. Enter 300 (nm) for both Channel A and Channel B Reference Wavelengths.
For a 900 Series Interface, you can choose events to set relays 1 through 7 on or off.
Another event, RVPRT, instructs the interface to read rack and vial information from the
attached autosampler at a specified time. For information about the instrument-timed events
for other supported instruments, refer to the documentation that came with the instrument.
In the Graphic Method Editor, you can insert instrument-timed events directly on the
chromatogram at a specified time. For more information, refer to Chapter10 of the
TotalChrom Workstation User’s Guide, Editing a Method and Results Graphically.
Introduction
This chapter describes the routine maintenance procedures required to keep your instrument
in proper working condition and to ensure the highest possible level of performance. It
includes maintenance checks that should be done on a daily basis and maintenance
procedures that should be done periodically depending on instrument use. This chapter is
divided into several sections, each section covering maintenance procedures for a particular
component of the system.
You should perform only the maintenance procedures described in this chapter. If additional
maintenance is required, contact a PerkinElmer Service Engineer.
Maintenance Procedures
This chapter contains the information needed to keep the Flexar PDA Detector in optimal
operating condition. With proper care and adherence to good chromatographic principles, the
Flexar PDA Detector will give you the high sensitivity and operating versatility it was designed
to provide. This maintenance chapter covers the following areas:
NOTE: Before calling for assistance, review the information and troubleshooting methods described
in this chapter. Service calls and downtime can often be minimized by a systematic approach
that will identify what may be a simple problem.
There are several routine maintenance checks that should be made from time to time in
order to determine if noise, drift, and general performance are acceptable. The procedure
outlined here takes the user through a step-by-step maintenance check.
It must be remembered that the Flexar PDA Detector is just a single component in a
complete HPLC system. Though they may manifest themselves in the detector's output,
problems such as baseline instability can also be caused by leaky pumps and contaminated
columns and injection valves. Each component must be isolated and checked individually to
determine its contribution, if any, to the observed problem. The tests below assume that the
user is reasonably certain that other system components are operating properly.
58 . Flexar PDA LC Detector
Maintenance Guidelines
You can achieve long and trouble-free performance from your Flexar PDA Detector by
performing routine and preventive maintenance procedures. The frequency of maintenance
required will be determined by the amount of use the system receives, the cleanliness of the
environment, and the number and nature of the samples being analyzed.
Preventive Maintenance
Preventive maintenance ensures that your Detector will perform consistently at an optimal
level. To maintain the detector in 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.
Routine Maintenance
In addition to preventive maintenance, you can perform routine maintenance on the
detector, as needed, to keep it in proper working condition. Routine maintenance consists of
replacing the normal wear items such as the deuterium lamp and columns, whenever you
notice a degradation in performance. The exit window behind the flow cell should be
removed and cleaned periodically.
PerkinElmer replacement part numbers are referenced throughout this section; however,
when ordering replacements, refer to the HPLC Supplies Catalog or to a PerkinElmer Product
Description List.
To save time and money, refer to the Troubleshooting Guide in this chapter before
performing any service. Use the Troubleshooting Guide to pinpoint the problem, then follow
the suggested solutions.
NOTE: For maintenance procedures that require removing the chassis from the external cover, use
the Allen key tool which can be stored inside the instrument, above the “Chassis removal
tool” label. The shaft of the tool is placed between the chassis and the cover, behind the
bulkhead for the plumbing unions on the left side of the instrument. The handle of the tool is
pointed down, between the two unions.
Maintenance . 59
Lamps
The Flexar PDA Detector uses a deuterium lamp and/or a tungsten halogen lamp as light
sources.
WARNING
WARNING
60 . Flexar PDA LC Detector
Deuterium Lamp
(inside mount)
Tungsten Lamp
Ultraviolet Source
The ultraviolet source produces an intense, stable light by maintaining an electric arc in a
deuterium atmosphere. This emitted light is a continuous wavelength spectrum from 190 nm
to 400 nm.
Due to varying operating conditions, the useful life of a deuterium lamp can not be precisely
determined. However, when the lamp intensity decreases to 50% of the original output the
lamp has reached the end of its useful life. The deuterium lamps used are guaranteed for
500 hours of operation. If the lamp fails within that time, it will be replaced free of charge. If
the lamp fails within the next 500 hours, it will be replaced on a pro-rated basis.
If the deuterium lamp appears to be emitting low energy, you should eliminate all other
possible causes of low sensitivity before replacing the lamp.
Tools Required
To replace the deuterium lamp (see Figure 8), you need a 3/32-in. hex driver.
WARNING
1. Stop the pump if it is running, turn off power to the detector, and disconnect the flow
cell connections. Then disconnect the detector power cord from the rear panel of the
detector.
2. Remove the flow cell cover plate by loosening the four knurled securing screws.
Remove the flow cell by loosening the knurled screw at the base of the cell carriage and
sliding it out of the instrument.
3. Visually check the flow cell and make sure that there are no air bubbles in the cells, or
cracks in the cell windows, that will interfere with test procedures. These factors can
contribute to low lamp energy.
4. Allow enough time for the deuterium lamp and the lamp housing to thoroughly cool.
6. Loosen and remove the two #6 screws that hold the deuterium lamp to the housing
using the 3/32-in. hex driver, and remove the lamp.
7. The deuterium lamp contains a mercury timer switch. Remove the timer switch from the
lamp assembly as shown in Figure 9 and dispose of it properly.
Maintenance . 63
Deuterium Lamp
Deuterium Lamp
(r emoved from mo unt)
8. Install the new deuterium lamp and then reconnect the electrical power leads.
Tools Required
To replace the tungsten lamp (see Figure 8), the following tools are needed:
Replacement Procedure
The lamp is held by a top-cap assembly as well as two leads. To replace the tungsten lamp
follow this procedure:
1. Stop the pump if it is running and turn off power to the detector.
3. Disconnect the detector power cord from the rear panel of the detector.
4. Remove the flow cell cover plate by loosening the four knurled securing screws. Then
remove the flow cell by loosening the knurled screw at the base of the cell carriage and
sliding it out of the instrument.
5. Remove the top cover of the detector by loosening and then removing the four cabinet
screws and sliding the instrument cover forward. Remove the cell focus mirror cover by
loosening the two 3/32-in. hex screws.
6. Visually check the flow cell and make sure that there are no air bubbles in the cells or
cracks in the cell windows that will interfere with test procedures.
7. Using a 0.050-in. hex-key wrench, loosen the setscrew on the side of the lamp cap.
Slide the cap up and off the post.
9. Grasp the new bulb in its protective bag and cut off the bottom of the bag, thereby
exposing the contacts.
Deuterium Lamp
(inside mount)
Tungsten Lamp
10. Line up the leads with the receptacle contacts in the holder and push the bulb into
place. There is no particular polarity needed for the bulb.
11. Slide the cap back down over the new lamp, and allow the lamp to seek it’s own center.
12. Rotate the lamp cap until the lamp is vertical and secure the lamp by tightening the
setscrew. Then check to make sure that the lamp is held securely by the lamp cap.
13. Turn on the detector power switch and the VIS power switch.
14. Refer to Figure 11 and use a white piece of paper or card (business cards are ideal) to
check if the light image falls on the center of the cell focus mirror. If it doesn't, you
must loosen the setscrew (see Step 12) and adjust the bulb's position to achieve proper
alignment. Then retighten the setscrew.
Field Stop
MM1-2
Figure 11 Aligning the beam at the center of the cell focus mirror
15. Turn off the detector power and replace the cell focus mirror cover and the detector
cover.
Index
GLP ............................................................... 25
9 LEDs
functionality ................................................... 37
900 Series Interface status ............................................................ 37
timed events...................................................54 liquid chromatograph
autosampler parameters, setting ..................... 48
A detector parameters, setting ........................... 53
D Quality Control.................................................... 25
Decontamination .................................................22
S
detector, LC
setting parameters ..........................................53 Safety
Suitability test ................................................ 25
E Summary ......................................................... 8
Safety Information .............................................. 17
Electrical electrical safety .............................................. 19
outlet configurations........................................44 environmental conditions ................................ 18
requirements ..................................................44 solvent gradient program, creating....................... 51
Safety ............................................................19 Solvents ............................................................. 27
ElectroMagnetic Compatibility ...............................23 Auto-Ignition Temperature.............................. 28
Environmental Conditions ............................... 18, 33 HPLC grade solvents ....................................... 34
labeling.......................................................... 50
F Low boiling points .......................................... 27
Specifications...................................................... 40
Fuses ..................................................................44 Start-up Kit......................................................... 43
Storage Conditions .............................................. 18
I System Description
specifications.................................................. 40
Installation
electrical requirements ....................................44
required air quality ..........................................33 T
Summary........................................................43 timed events
IPV .....................................................................25 programming ................................................. 54
Instrument Specifications .....................................40 TotalChrom connections ...................................... 47
instrument, timed events setting ..........................54
W
L
Warnings
Labels on the instrument......................................24 Hazardous Chemical ....................................... 26
Labels, Warning Signs ..........................................13 Waste and Solvent Disposal ................................. 34
Laboratory WEEE Instructions............................................... 21
relative humidity .............................................33
Laboratory Practices
68 . Flexar PDA LC Detector