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Waters Post-Column

Reaction Module
Installation Guide
71500017204/Revision B

Copyright © Waters Corporation 2010


All rights reserved
Copyright notice
© 2010 WATERS CORPORATION. PRINTED IN THE UNITED STATES OF
AMERICA AND IN IRELAND. ALL RIGHTS RESERVED. THIS
DOCUMENT OR PARTS THEREOF MAY NOT BE REPRODUCED IN ANY
FORM WITHOUT THE WRITTEN PERMISSION OF THE PUBLISHER.
The information in this document is subject to change without notice and
should not be construed as a commitment by Waters Corporation. Waters
Corporation assumes no responsibility for any errors that may appear in this
document. This document is believed to be complete and accurate at the time
of publication. In no event shall Waters Corporation be liable for incidental or
consequential damages in connection with, or arising from, its use.

Trademarks
Millennium and Waters are registered trademarks of Waters Corporation,
and “THE SCIENCE OF WHAT’S POSSIBLE.” is a trademark of Waters
Corporation.
Other registered trademarks or trademarks are the sole property of their
owners.

ii
Customer comments
Waters’ Technical Communications department invites you to tell us of any
errors you encounter in this document or to suggest ideas for otherwise
improving it. Please help us better understand what you expect from our
documentation so that we can continuously improve its accuracy and
usability.
We seriously consider every customer comment we receive. You can reach us
at tech_comm@waters.com.

Contacting Waters
®
Contact Waters with enhancement requests or technical questions regarding
the use, transportation, removal, or disposal of any Waters product. You can
reach us via the Internet, telephone, or conventional mail.

Waters contact information

Contacting medium Information


Internet The Waters Web site includes contact
information for Waters locations worldwide.
Visit www.waters.com.
Telephone and fax From the USA or Canada, phone 800
252-HPLC, or fax 508 872 1990.
For other locations worldwide, phone and fax
numbers appear in the Waters Web site.
Conventional mail Waters Corporation
34 Maple Street
Milford, MA 01757
USA

iii
Safety considerations
Some reagents and samples used with Waters instruments and devices can
pose chemical, biological, and radiological hazards. You must know the
potentially hazardous effects of all substances you work with. Always follow
Good Laboratory Practice, and consult your organization’s safety
representative for guidance.

Safety advisories
Consult Appendix A for a comprehensive list of warning and caution
advisories.

Operating this instrument


When operating this instrument, follow standard quality-control (QC)
procedures and the guidelines presented in this section.

Applicable symbols

Symbol Definition

Manufacturer location

Authorized representative of the European


Community
Confirms that a manufactured product complies
with all applicable European Community
directives

Australia C-Tick EMC Compliant

Confirms that a manufactured product complies


with all applicable United States and Canadian
safety requirements

Consult instructions for use

iv
Audience and purpose
This guide is intended for personnel who install the Waters Post-Column
Reaction Module.

Intended use of the Waters Post-Column Reaction Module


The Waters Alliance Post-Column Reaction Module is for research use only.

Calibrating
To calibrate LC systems, follow acceptable calibration methods using at least
five standards to generate a standard curve. The concentration range for
standards should include the entire range of QC samples, typical specimens,
and atypical specimens.
When calibrating mass spectrometers, consult the calibration section of the
operator’s guide for the instrument you are calibrating. In cases where an
overview and maintenance guide, not operator’s guide, accompanies the
instrument, consult the instrument’s online Help system for calibration
instructions.

Quality-control
Routinely run three QC samples that represent subnormal, normal, and
above-normal levels of a compound. Ensure that QC sample results fall within
an acceptable range, and evaluate precision from day to day and run to run.
Data collected when QC samples are out of range might not be valid. Do not
report these data until you are certain that the instrument performs
satisfactorily.

ISM classification

ISM Classification: ISM Group 1 Class B


This classification has been assigned in accordance with CISPR 11 Industrial
Scientific and Medical (ISM) instruments requirements. Group 1 products
apply to intentionally generated and/or used conductively coupled
radio-frequency energy that is necessary for the internal functioning of the
equipment. Class B products are suitable for use in both commercial and

v
residential locations and can be directly connected to a low voltage,
power-supply network.

EC authorized representative

Waters Corporation (Micromass UK Ltd.)


Floats Road
Wythenshawe
Manchester M23 9LZ
United Kingdom

Telephone: +44-161-946-2400
Fax: +44-161-946-2480
Contact: Quality manager

vi
Table of Contents
Copyright notice ................................................................................................... ii

Trademarks ............................................................................................................ ii
Customer comments ............................................................................................ iii

Contacting Waters ............................................................................................... iii

Safety considerations .......................................................................................... iv


Safety advisories ................................................................................................. iv

Operating this instrument ................................................................................. iv


Applicable symbols ............................................................................................. iv
Audience and purpose.......................................................................................... v
Intended use of the Waters Post-Column Reaction Module .............................. v
Calibrating ........................................................................................................... v
Quality-control ..................................................................................................... v

ISM classification .................................................................................................. v


ISM Classification: ISM Group 1 Class B .......................................................... v

EC authorized representative ........................................................................... vi

1 Introduction ............................................................................................ 1-1


Design features .................................................................................................. 1-2

RXN 1000 reaction coil ..................................................................................... 1-3

CHEX countercurrent heat exchanger ........................................................ 1-3

2 Installing the Post-Column Reaction Module ................................. 2-1


Selecting the site ............................................................................................... 2-2

Unpacking the PCRM ....................................................................................... 2-2


Electrical connections ..................................................................................... 2-3
Selecting PCRM voltage .................................................................................. 2-4
Making electrical connections ......................................................................... 2-4

Table of Contents vii


Making fluidic connections ............................................................................ 2-5

3 Operating the Post-Column Reaction Module ................................ 3-1


Powering up the PCRM ................................................................................... 3-2

Operating the PCRM ........................................................................................ 3-2


Correcting an erroneous entry ........................................................................ 3-3
Reentering control mode.................................................................................. 3-3
Turning off the Post-Column Reaction Module.............................................. 3-3
Checking the temperature setting .................................................................. 3-3
Shutting down the temperature limit............................................................. 3-4

Equilibrating the PCRM .................................................................................. 3-4

A Safety Advisories .................................................................................. A-1


Warning symbols ............................................................................................... A-2
Task-specific hazard warnings........................................................................ A-2
Specific warnings ............................................................................................. A-3

Caution symbol .................................................................................................. A-5

Warnings that apply to all Waters instruments ......................................... A-6

Electrical and handling symbols ................................................................. A-12


Electrical symbols .......................................................................................... A-12
Handling symbols .......................................................................................... A-13

B Specifications ........................................................................................ B-1

C Warranty and Service Information .................................................. C-1


Limited product warranty ............................................................................. C-2
Warranty service.............................................................................................. C-2
Warranty service exceptions ........................................................................... C-3
Warranty period............................................................................................... C-3

Ordering information ..................................................................................... C-4


Where to place orders ...................................................................................... C-4
How to place orders ......................................................................................... C-4
Part numbers .................................................................................................. C-5

viii Table of Contents


Pricing .............................................................................................................. C-5
Payment terms................................................................................................. C-5

Shipments, damages, claims, and returns .................................................. C-5


Shipments ........................................................................................................ C-5
Damages ........................................................................................................... C-5
Claims............................................................................................................... C-6
Returns ............................................................................................................. C-6

D RXN 1000 Coil Care and Use .............................................................. D-1


Introduction ...................................................................................................... D-2

RXN coil materials of construction/specifications ................................... D-2

Installation ........................................................................................................ D-2

Helpful hints and precautions ...................................................................... D-4

Ordering information ..................................................................................... D-5

E System Startup Kit List ...................................................................... E-1

Index ..................................................................................................... Index-1

Table of Contents ix
x Table of Contents
1 Introduction

Contents

Topic Page
Design features 1-2
RXN 1000 reaction coil 1-3
CHEX countercurrent heat exchanger 1-3

1-1
Design features
The Waters® Post-Column Reaction Module (PCRM) is shown below.

Post-Column reaction module

TP01695

There are four bulkhead fittings on the front panel of the module. Three
bulkhead fittings provide fluidic paths into a two-stage, Post-Column Reaction
Module. The fourth bulkhead fitting provides a fluidic path out of the module
to a detector. (Refer to Figure C-1 for information about using the PCRM for
applications requiring a one-stage reaction.)
The post-column reaction module includes an oven containing a RXN™ 1000
Reaction Coil and a CHEX™ Countercurrent Heat Exchanger.
Tip: The Waters Temperature Control Module is required for operating the
PCRM.
The analytical column is maintained in a separate column heater. Each
analyte exiting the column is prewarmed as it passes through the
Countercurrent Heat Exchanger (CHEX) to the post-column reactor oven.
At the first junction inside the reactor oven, the column effluent merges with a
stream of reagent solution that has also been preheated by passage through
the CHEX unit. The two streams mix and pass through the RXN 1000
Reaction Coil where the 1-mL volume coil is maintained at constant
temperature to cause the desired reaction.
After exiting the coil, the effluent immediately enters a second junction where
it merges with a second pre-warmed reagent solution if a secondary
post-column reaction is desired. The fluid stream leaves the oven, is cooled to
ambient temperature by passing through the CHEX unit, and then passes out
of the Post-Column Reaction Module and into the detector cell.

1-2 Introduction
RXN 1000 reaction coil
A knitted open tubular design has been used to create one milliliter of reactor
volume with minimal bandspreading in a compact linear shape. This RXN
1000 Reaction Coil is constructed of 0.018-in. ID PTFE using a series of tight
180° turns with each successive turn 90° out-of-plane. The effect of this
method of construction is to cause effective mixing or turbulence in the radial
direction while disrupting the laminar flow profile which would otherwise lead
to significant axial broadening of the chromatographic bands in an open tube
of this internal diameter.

Waters RXN 1000 reaction coil design

~180° turns,
~90° out-of-plane

Waters RXN™ 1000 Coil

TP01710

CHEX countercurrent heat exchanger


The CHEX Countercurrent Heat Exchanger performs several tasks
concurrently. As shown in the figure below, post-column reagents 1 and 2 as
well as the effluent from the HPLC column pass in parallel through the CHEX
unit into the post-column reactor. The total flow of these three streams is

RXN 1000 reaction coil 1-3


balanced by the countercurrent flow of the reactor effluent which passes back
through the CHEX unit on its way to the detector.

CHEX countercurrent heat exchanger design

Reagent 1
Solder sheath
over copperplate

Reagent 2
Steel wire wrap
over stainless steel
tubing
Column out

Reactor out

Because of the intimate thermal contact between the fluid paths, the heat
from the reactor effluent is transferred to the incoming streams, thereby
prewarming the reactants for more uniform reactions. At the same time, the
reactor effluent is cooled to nearly ambient temperature which not only
improves detector performance but also protects the reagent solution and the
possibly unstable derivatives, once formed, from thermal degradation.
For example, in carbamate analysis exposing the reagent solution to excessive
heat results in a higher level of background fluorescence appearing as
baseline noise. Also, the isoindole derivative can be destroyed by heat and
light. Thus, cooling the reactor effluent quickly maximizes the amount of
derivative that reaches the detector cell while minimizing background
fluorescence, thereby ultimately lowering the limit of detection.

1-4 Introduction
2 Installing the Post-Column
Reaction Module

Contents

Topic Page
Selecting the site 2-2
Unpacking the PCRM 2-2
Electrical connections 2-3
Making fluidic connections 2-5

2-1
Selecting the site
The module contains solvent drains to direct solvent away from the unit in the
event of a leak. The module should be installed on a level surface to insure
proper drainage.
Install the Post-Column Reaction Module in an area free from extremes of
temperature, humidity, appreciable shock, and vibration. Make sure the
system is connected to a properly grounded power source that is free of
transients and fluctuation.

Unpacking the PCRM


The Waters® Post-Column Reaction Module is shipped in one carton that
contains the following items:
• Waters Post-Column Reaction Module
• Post-Column Reaction Module Startup Kit (see the Startup Kit List for a
list of contents)
• Certificate of Validation
• Installation Manual
Before opening the shipping container, inspect it for damage or evidence of
mishandling. If it has been damaged or mishandled, notify the carrier before
opening the container. See Appendix C for more information.
Tip: Save the shipping container for future use.

To unpack the module:


1. Open the carton and remove the Startup Kit and other items from the
slot at one end of the carton.
2. Using both hands, lift the module and its foam packing material out of
the carton.
3. Carefully set the module down, then remove the foam packing material
from the ends of the unit.
4. Check the contents of the Startup Kit against the Startup Kit parts list
to confirm that all items are included.

2-2 Installing the Post-Column Reaction Module


5. Verify that the serial number on the back of the module matches the
serial number on the Certificate of Validation. Keep the Certificate of
Validation for future reference.
For more information about the warranty, refer to Appendix C.
6. Inspect all items for damage. Immediately report any shipping damage
to both the shipping company and your Waters representative. Contact
Waters Technical Service at 800-252-4752, U.S. and Canadian
customers only. Other customers, call your local Waters subsidiary, or
call Waters corporate headquarters at 508-478-2000 (U.S.A.). Refer to
Appendix C, for complete information on reporting shipping damages
and submitting claims.

Electrical connections

PCRM electrical controls and connections

Power switch

Temperature
control cable Fuse socket

Line cord Voltage TP01693


connector selection
switch

Electrical connections 2-3


Selecting PCRM voltage
The PCRM can be adjusted to operate at the two nominal voltages listed in the
table below.

PCRM voltage ranges and fuse ratings

Nominal voltage Frequency range Fuse rating


115 Vac 60 Hz (57-63) 2.5 A
230 Vac 50 Hz (47-53) 1.25 A

To select the desired voltage on the PCRM:


1. Make sure that the PCRM power switch is Off. Disconnect the power
cord.
2. Reposition the voltage selection switch (red switch, see figure “PCRM
electrical controls and connections” on page 2-3 for location) with a
flat-head screwdriver so that the desired voltage is displayed.
3. The fuse socket is located on the side of the PCRM near the rear (see
figure “PCRM electrical controls and connections” on page 2-3). Remove
the cover with a flat-head screwdriver.
4. Install a properly rated fuse as specified in table titled “PCRM voltage
ranges and fuse ratings” on page 2-4. Replace the fuse receptacle cover
using a flat-head screwdriver.
5. Connect the power cord. Turn the module On when you are ready to
perform an analysis.

Making electrical connections


Make the following PCRM electrical connections:
1. Connect the 9-pin connector of the temperature control cable that is
attached to the PCRM to any of the three external device connectors on a
Temperature Control Module (TCM) rear panel and tighten the screws.
2. Connect a power cord to the PCRM. Connect the other end into a power
supply outlet which meets the requirements in table titled “PCRM
voltage ranges and fuse ratings” on page 2-4.

2-4 Installing the Post-Column Reaction Module


Making fluidic connections
Connect the inlet tubing provided with the Post-Column Reaction Module as
shown in figure “PCRM electrical controls and connections” on page 2-3 to
ensure proper operation.

PCRM fluidic connections

Connect to
reagent pump 1 from
Pump 1 from
bulkhead fitting Pump 2 to
Detector from
(Yellow) Column

Connect to
reagent pump 2 Waters
Post C
bulkhead fitting olumn
Reactio
n Mod
ule
(Green)
Connect to
detector inlet
fitting (Blue) Connect
Connect to to waste
column outlet reservoir TP01701
(Red)

To connect the tubing to the bulkhead fittings on the PCRM:


1. Connect the tubing (color coded red) from the outlet connection of the
analytical column to the bulkhead fitting labeled “from Column.”
2. Connect the tubing (color coded yellow) from the outlet connector of the
reagent pump delivering reagent 1 to the bulkhead fitting labeled “from
Pump 1”
3. Connect the tubing (color coded green) from the outlet connector of the
reagent pump delivering reagent 2 to the bulkhead fitting labeled “from
Pump 2.”
4. Connect the tubing (color coded blue) from the bulkhead fitting labeled
“to Detector” to the inlet of the detector cell.
5. Connect the tubing from the drip tray outlet to the waste reservoir.

Making fluidic connections 2-5


2-6 Installing the Post-Column Reaction Module
3 Operating the Post-Column
Reaction Module
.
Contents

Topic Page
Powering up the PCRM 3-2
Operating the PCRM 3-2
Equilibrating the PCRM 3-4

3-1
Powering up the PCRM
Power up the PCRM and any devices connected to the data system as follows:
Tip: Refer to the installation guides for each device for powerup procedures.
1. Power up all the equipment not controlled by the data system.
2. Power up the Post-Column Reaction Module, the Temperature Control
Module (TCM), and all other equipment controlled through the
IEEE-488 bus.
3. Power up the printer and the monitor.
4. Power up the computer.

Operating the PCRM


Tip: Make sure the selected operating temperature is compatible with the
solvent(s) used.

To operate the Post-Column Reaction Module:


1. Turn the power switch of the PCRM to 1 (On).
2. Turn the ON/OFF switch on the TCM to On - 1. The TCM undergoes a
brief self-test routine, then enters Control mode.
3. Press any key to enter Input mode.
4. If more than one module is connected, make sure that you select the
proper unit number. Press SELECT, then enter the number (1-3) of the
module. The corresponding SELECT UNIT LED illuminates. The
TEMPERATURE display shows the measured temperature for that
module.
Tip: The preset values are ambient for the lower limit and 120°C for the
upper limit for the Post-Column Reaction. Setting a temperature outside
prescribed limits may cause the alarm to trigger.
5. Press SET, then enter the desired operating temperature in degrees and
tenths of degrees, then press ENTER. The display responds by showing
the measured temperature for that channel. The TCM then begins to
control that channel.

3-2 Operating the Post-Column Reaction Module


Tip: Refer to the Waters documentation for information about
temperature settings for your application.
6. If you want to set the temperature for another module, repeat the
procedure from step 2.
Tip: Over or Under temperature limits should not be set until the
module unit has equilibrated to temperature.
To reset the system, follow the procedure described in Shutting Down the
Temperature Limit at the end of this section.

Correcting an erroneous entry


If you make a mistake in entering temperature values and have not yet
pressed ENTER, press CLEAR. The TEMPERATURE display then reverts to
the value originally displayed for that parameter. Enter the new value and
press ENTER.
If you have already pressed ENTER, press the number of the unit, then the
key corresponding to the parameter containing the error. Enter the corrected
value, then press ENTER.

Reentering control mode


When you have finished programming the TCM, press ENTER. The unit
automatically reverts to Control mode in 5 seconds or when ENTER is
pressed. The TCM executes the parameters programmed into it in Input mode
and resumes its scan of the three channels.

Turning off the Post-Column Reaction Module


To turn the Post-Column Reaction Module off:
1. Press SELECT and the number of the module which you wish to turn
off.
2. Press Set, CLEAR, and then ENTER. The Post-Column Reaction turns
off and the TEMPERATURE display reads OFF for that channel.

Checking the temperature setting


If you wish to check the set or limit temperature of a Post-Column Reaction
during operation, select the number of the unit you want to check, then press

Operating the PCRM 3-3


the desired temperature parameter (OVER, UNDER, or SET). The
TEMPERATURE display shows the desired parameter, then reverts to
scanning all connected units after 5 seconds.
If a channel is not connected to a module, the TEMPERATURE display shows
the status message UC (unconnected). If a device is connected but is not
turned on, the TEMPERATURE display reads OFF.

Shutting down the temperature limit


If the actual temperature of a Post-Column Reaction Module exceeds the
OVER temperature limit, the PCRM automatically shuts that channel off and
sounds the alarm. The OVER LED then illuminates. If the temperature of
the module falls below the UNDER temperature limit, the alarm sounds, but
the PCRM does not shut the module off. The alarm continues to sound until
the condition is corrected.
To reset the PCRM after a limit shutdown, check the set temperature and
both limits, then correct the problem or enter new values.

Equilibrating the PCRM


Allow 1 hour for the Post-Column Reaction Module to stabilize at any set
temperature.
Tip: Reaction times vary with temperature. Adequate time must be provided
for temperature equilibration.

3-4 Operating the Post-Column Reaction Module


A Safety Advisories

Waters instruments display hazard symbols designed to alert you to the


hidden dangers of operating and maintaining the instruments. Their
corresponding user guides also include the hazard symbols, with
accompanying text statements describing the hazards and telling you
how to avoid them. This appendix presents all the safety symbols and
statements that apply to the entire line of Waters products.

Contents

Topic Page
Warning symbols A-2
Caution symbol A-5
Warnings that apply to all Waters instruments A-6
Electrical and handling symbols A-12

A-1
Warning symbols
Warning symbols alert you to the risk of death, injury, or seriously adverse
physiological reactions associated with an instrument’s use or misuse. Heed
all warnings when you install, repair, and operate Waters instruments.
Waters assumes no liability for the failure of those who install, repair, or
operate its instruments to comply with any safety precaution.

Task-specific hazard warnings


The following warning symbols alert you to risks that can arise when you
operate or maintain an instrument or instrument component. Such risks
include burn injuries, electric shocks, ultraviolet radiation exposures, and
others.
When the following symbols appear in a manual’s narratives or procedures,
their accompanying text identifies the specific risk and explains how to avoid
it.

Warning: (General risk of danger. When this symbol appears on an


instrument, consult the instrument’s user documentation for important
safety-related information before you use the instrument.)

Warning: (Risk of burn injury from contacting hot surfaces.)

Warning: (Risk of electric shock.)

Warning: (Risk of fire.)

Warning: (Risk of sharp-point puncture injury.)

Warning: (Risk of hand crush injury.)

Warning: (Risk of exposure to ultraviolet radiation.)

Warning: (Risk of contacting corrosive substances.)

Warning: (Risk of exposure to a toxic substance.)

Warning: (Risk of personal exposure to laser radiation.)

A-2 Safety Advisories


Warning: (Risk of exposure to biological agents that can pose a serious
health threat.)

Warning: (Risk of tipping.)

Warning: (Risk of explosion.)

Warning: (Risk of eye injury.)

Specific warnings
The following warnings can appear in the user manuals of particular
instruments and on labels affixed to them or their component parts.

Burst warning
This warning applies to Waters instruments fitted with nonmetallic tubing.

Warning: Pressurized nonmetallic, or polymer, tubing can burst.


Observe these precautions when working around such tubing:
• Wear eye protection.
• Extinguish all nearby flames.
• Do not use tubing that is, or has been, stressed or kinked.
• Do not expose nonmetallic tubing to incompatible compounds like
tetrahydrofuran (THF) and nitric or sulfuric acids.
• Be aware that some compounds, like methylene chloride and
dimethyl sulfoxide, can cause nonmetallic tubing to swell, which
significantly reduces the pressure at which the tubing can rupture.

Warning symbols A-3


Mass spectrometer flammable solvents warning
This warning applies to instruments operated with flammable solvents.

Warning: Where significant quantities of flammable solvents are


involved, a continuous flow of nitrogen into the ion source is required to
prevent possible ignition in that enclosed space.
Ensure that the nitrogen supply pressure never falls below 690 kPa
(6.9 bar, 100 psi) during an analysis in which flammable solvents are
used. Also ensure a gas-fail connection is connected to the LC system so
that the LC solvent flow stops if the nitrogen supply fails.

Mass spectrometer shock hazard


This warning applies to all Waters mass spectrometers.

Warning: To avoid electric shock, do not remove the mass spectrometer’s


protective panels. The components they cover are not user-serviceable.

This warning applies to certain instruments when they are in Operate mode.

Warning: High voltages can be present at certain external surfaces of


the mass spectrometer when the instrument is in Operate mode. To
avoid non-lethal electric shock, make sure the instrument is in Standby
mode before touching areas marked with this high voltage warning
symbol.

A-4 Safety Advisories


Biohazard warning
This warning applies to Waters instruments that can be used to process
material that might contain biohazards: substances that contain biological
agents capable of producing harmful effects in humans.

Warning: Waters instruments and software can be used to analyze or


process potentially infectious human-sourced products, inactivated
microorganisms, and other biological materials. To avoid infection with
these agents, assume that all biological fluids are infectious, observe
Good Laboratory Practices, and consult your organization’s biohazard
safety representative regarding their proper use and handling. Specific
precautions appear in the latest edition of the US National Institutes of
Health (NIH) publication, Biosafety in Microbiological and Biomedical
Laboratories (BMBL).

Chemical hazard warning


This warning applies to Waters instruments that can process corrosive, toxic,
flammable, or other types of hazardous material.

Warning: Waters instruments can be used to analyze or


process potentially hazardous substances. To avoid injury
with any of these materials, familiarize yourself with the
materials and their hazards, observe Good Laboratory
Practices (GLP), and consult your organization’s safety
representative regarding proper use and handling.
Guidelines are provided in the latest edition of the National
Research Council's publication, Prudent Practices in the
Laboratory: Handling and Disposal of Chemicals.

Caution symbol
The caution symbol signifies that an instrument’s use or misuse can damage
the instrument or compromise a sample’s integrity. The following symbol and
its associated statement are typical of the kind that alert you to the risk of
damaging the instrument or sample.

Caution: To avoid damage, do not use abrasives or solvents to clean the


instrument’s case.

Caution symbol A-5


Warnings that apply to all Waters instruments
When operating this device, follow standard quality control procedures and
the equipment guidelines in this section.

Attention: Changes or modifications to this unit not expressly approved by the


party responsible for compliance could void the user’s authority to operate the
equipment.

Important: Toute modification sur cette unité n’ayant pas été expressément
approuvée par l’autorité responsable de la conformité à la réglementation peut
annuler le droit de l’utilisateur à exploiter l’équipement.

Achtung: Jedwede Änderungen oder Modifikationen an dem Gerät ohne die


ausdrückliche Genehmigung der für die ordnungsgemäße Funktionstüchtigkeit
verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des
Systems führen.

Avvertenza: qualsiasi modifica o alterazione apportata a questa unità e non


espressamente autorizzata dai responsabili per la conformità fa decadere il
diritto all'utilizzo dell'apparecchiatura da parte dell'utente.

Atencion: cualquier cambio o modificación efectuado en esta unidad que no


haya sido expresamente aprobado por la parte responsable del cumplimiento
puede anular la autorización del usuario para utilizar el equipo.

注意:未經有關法規認證部門允許對本設備進行的改變或修改,可能會使使用者喪失操作該設
備的權利。

注意:未经有关法规认证部门明确允许对本设备进行的改变或改装,可能会使使用者丧失操
作该设备的合法性。

주의: 규정 준수를 책임지는 당사자의 명백한 승인 없이 이 장치를 개조 또는 변경할 경우,


이 장치를 운용할 수 있는 사용자 권한의 효력을 상실할 수 있습니다.

注意:規制機関から明確な承認を受けずに本装置の変更や改造を行うと、本装置のユー
ザーとしての承認が無効になる可能性があります。

A-6 Safety Advisories


Warning: Use caution when working with any polymer tubing under pressure:
• Always wear eye protection when near pressurized polymer tubing.
• Extinguish all nearby flames.
• Do not use tubing that has been severely stressed or kinked.
• Do not use nonmetallic tubing with tetrahydrofuran (THF) or concentrated
nitric or sulfuric acids.
• Be aware that methylene chloride and dimethyl sulfoxide cause nonmetallic
tubing to swell, which greatly reduces the rupture pressure of the tubing.
Attention: Manipulez les tubes en polymère sous pression avec precaution:
• Portez systématiquement des lunettes de protection lorsque vous vous
trouvez à proximité de tubes en polymère pressurisés.
• Eteignez toute flamme se trouvant à proximité de l’instrument.
• Evitez d'utiliser des tubes sévèrement déformés ou endommagés.
• Evitez d'utiliser des tubes non métalliques avec du tétrahydrofurane (THF)
ou de l'acide sulfurique ou nitrique concentré.
• Sachez que le chlorure de méthylène et le diméthylesulfoxyde entraînent le
gonflement des tuyaux non métalliques, ce qui réduit considérablement leur
pression de rupture.
Vorsicht: Bei der Arbeit mit Polymerschläuchen unter Druck ist besondere
Vorsicht angebracht:
• In der Nähe von unter Druck stehenden Polymerschläuchen stets
Schutzbrille tragen.
• Alle offenen Flammen in der Nähe löschen.
• Keine Schläuche verwenden, die stark geknickt oder überbeansprucht sind.
• Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder
konzentrierte Salpeter- oder Schwefelsäure verwenden.
• Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische
Schläuche quellen; dadurch wird der Berstdruck des Schlauches erheblich
reduziert.

Warnings that apply to all Waters instruments A-7


Attenzione: fare attenzione quando si utilizzano tubi in materiale polimerico
sotto pressione:
• Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero
pressurizzati.
• Spegnere tutte le fiamme vive nell'ambiente circostante.
• Non utilizzare tubi eccessivamente logorati o piegati.
• Non utilizzare tubi non metallici con tetraidrofurano (THF) o acido solforico
o nitrico concentrati.
• Tenere presente che il cloruro di metilene e il dimetilsolfossido provocano
rigonfiamenti nei tubi non metallici, riducendo notevolmente la pressione di
rottura dei tubi stessi.
Advertencia: se recomienda precaución cuando se trabaje con tubos de
polímero sometidos a presión:
• El usuario deberá protegerse siempre los ojos cuando trabaje cerca de tubos
de polímero sometidos a presión.
• Si hubiera alguna llama las proximidades.
• No se debe trabajar con tubos que se hayan doblado o sometido a altas
presiones.
• Es necesario utilizar tubos de metal cuando se trabaje con tetrahidrofurano
(THF) o ácidos nítrico o sulfúrico concentrados.
• Hay que tener en cuenta que el cloruro de metileno y el sulfóxido de dimetilo
dilatan los tubos no metálicos, lo que reduce la presión de ruptura de los
tubos.

警告:當在有壓力的情況下使用聚合物管線時,小心注意以下幾點。
• 當接近有壓力的聚合物管線時一定要戴防護眼鏡。
• 熄滅附近所有的火焰。
• 不要使用已經被壓癟或嚴重彎曲管線。
• 不要在非金屬管線中使用四氫呋喃或濃硝酸或濃硫酸。
• 要了解使用二氯甲烷及二甲基亞楓會導致非金屬管線膨脹,大大降低管線的耐壓能力。

A-8 Safety Advisories


警告:当有压力的情况下使用管线时,小心注意以下几点:
• 当接近有压力的聚合物管线时一定要戴防护眼镜。
• 熄灭附近所有的火焰。
• 不要使用已经被压瘪或严重弯曲的管线。
• 不要在非金属管线中使用四氢呋喃或浓硝酸或浓硫酸。
• 要了解使用二氯甲烷及二甲基亚枫会导致非金属管线膨胀,大大降低管线的耐压能力。

경고: 가압 폴리머 튜브로 작업할 경우에는 주의하십시오.


• 가압 폴리머 튜브 근처에서는 항상 보호 안경을 착용하십시오.
• 근처의 화기를 모두 끄십시오.
• 심하게 변형되거나 꼬인 튜브는 사용하지 마십시오.
• 비금속(Nonmetallic) 튜브를 테트라히드로푸란(Tetrahydrofuran: THF) 또는
농축 질산 또는 황산과 함께 사용하지 마십시오.
• 염화 메틸렌(Methylene chloride) 및 디메틸술폭시드(Dimethyl sulfoxide)는
비금속 튜브를 부풀려 튜브의 파열 압력을 크게 감소시킬 수 있으므로 유의하십시오.

警告:圧力のかかったポリマーチューブを扱うときは、注意してください。
• 加圧されたポリマーチューブの付近では、必ず保護メガネを着用してください。
• 近くにある火を消してください。
• 著しく変形した、または折れ曲がったチューブは使用しないでください。
• 非金属チューブには、テトラヒドロフラン(THF)や高濃度の硝酸または硫酸などを流
さないでください。
• 塩化メチレンやジメチルスルホキシドは、非金属チューブの膨張を引き起こす場合が
あり、その場合、チューブは極めて低い圧力で破裂します。

Warnings that apply to all Waters instruments A-9


Warning: The user shall be made aware that if the equipment is used in a
manner not specified by the manufacturer, the protection provided by the
equipment may be impaired.

Attention: L’utilisateur doit être informé que si le matériel est utilisé d’une
façon non spécifiée par le fabricant, la protection assurée par le matériel risque
d’être défectueuses.

Vorsicht: Der Benutzer wird darauf aufmerksam gemacht, dass bei


unsachgemäßer Verwenddung des Gerätes die eingebauten
Sicherheitseinrichtungen unter Umständen nicht ordnungsgemäß
funktionieren.

Attenzione: si rende noto all'utente che l'eventuale utilizzo


dell'apparecchiatura secondo modalità non previste dal produttore può
compromettere la protezione offerta dall'apparecchiatura.

Advertencia: el usuario deberá saber que si el equipo se utiliza de forma


distinta a la especificada por el fabricante, las medidas de protección del equipo
podrían ser insuficientes.

警告:使用者必須非常清楚如果設備不是按照製造廠商指定的方式使用,那麼該設備所提供
的保護將被消弱。

警告:使用者必须非常清楚如果设备不是按照制造厂商指定的方式使用,那么该设备所提供
的保护将被削弱。

경고: 제조업체가 명시하지 않은 방식으로 장비를 사용할 경우 장비가 제공하는 보호 수단이


제대로 작동하지 않을 수 있다는 점을 사용자에게 반드시 인식시켜야 합니다.

警告: ユーザーは、製造元により指定されていない方法で機器を使用すると、機器が提供
している保証が無効になる可能性があることに注意して下さい。

A-10 Safety Advisories


Warning: To protect against fire, replace fuses with those of the type
and rating printed on panels adjacent to instrument fuse covers.
Attention: pour éviter tout risque d'incendie, remplacez toujours les
fusibles par d'autres du type et de la puissance indiqués sur le panneau
à proximité du couvercle de la boite à fusible de l'instrument.
Vorsicht: Zum Schutz gegen Feuer die Sicherungen nur mit
Sicherungen ersetzen, deren Typ und Nennwert auf den Tafeln neben
den Sicherungsabdeckungen des Geräts gedruckt sind.
Attenzione: per garantire protezione contro gli incendi, sostituire i
fusibili con altri dello stesso tipo aventi le caratteristiche indicate sui
pannelli adiacenti alla copertura fusibili dello strumento.
Advertencia: Para evitar incendios, sustituir los fusibles por aquellos
del tipo y características impresos en los paneles adyacentes a las
cubiertas de los fusibles del instrumento.

警告 : 為了避免火災,更換保險絲時,請使用與儀器保險絲蓋旁面板上所印刷之相同類
型與規格的保險絲。

警告 : 为了避免火灾,应更换与仪器保险丝盖旁边面板上印刷的类型和规格相同的
保险丝。

경고: 화재의 위험을 막으려면 기기 퓨즈 커버에 가까운 패널에 인쇄된 것과 동일한


타입 및 정격의 제품으로 퓨즈를 교체하십시오.

警告 : 火災予防のために、ヒューズ交換では機器ヒューズカバー脇のパネルに記
載されているタイプおよび定格のヒューズをご使用ください。

Warnings that apply to all Waters instruments A-11


Electrical and handling symbols

Electrical symbols
These can appear in instrument user manuals and on the instrument’s front
or rear panels.

Electrical power on

Electrical power off

Standby

Direct current

Alternating current

Protective conductor terminal

Frame, or chassis, terminal

Fuse

Recycle symbol: Do not dispose in municipal waste.

A-12 Safety Advisories


Handling symbols
These handling symbols and their associated text can appear on labels affixed
to the outer packaging of Waters instrument and component shipments.

Keep upright!

Keep dry!

Fragile!

Use no hooks!

Electrical and handling symbols A-13


A-14 Safety Advisories
B Specifications

Post-Column Reaction Module


Power consumption Nominal 20 W
Environmental Data Operating temperature: 10 to 40 °C
Storage temperature: 40 to 70 °C
Humidity: 10 to 90% non-condensing
Dimensions Length: 9.21 cm (3.625 inches)
Height: 58.42 cm (23.0 inches)
Width: 16.51 cm (6.5 inches)
Safety features Line fusing
Grounding
Solvent spill drainage
Overtemperature protection
Temperature Range Ambient to 120 °C
Maximum temperature 120 °C at 450 psi for 72 hours
Limit
Temperature Setpoint +/- 0.5 °C at 80 °C measured with
Accuracy temperature probe at designated point
Temperature Stability +/- 0.5 °C under identical conditions
Temperature +/- 0.1 °C from day to day
Repeatability
Mechanical Temperature 125 °C +/- 3.9 °C
Limit Switch

B-1
B-2 Specifications
C Warranty and Service
Information

Contents

Topic Page
Limited product warranty C-2
Ordering information C-4
Shipments, damages, claims, and returns C-5

C-1
Limited product warranty
®
Waters Corporation, provides this limited warranty (the Warranty) to protect
customers from nonconformity in the product workmanship or materials. The
Warranty covers all new products manufactured by Waters and its
subsidiaries.
The Warranty is as follows:
Waters warrants that all products sold by them will be of good quality and
workmanship. The products will be fit for their intended purpose(s) when used
strictly in accordance with Waters instructions for use during the applicable
warranty period.
The foregoing warranty is exclusive and in lieu of all other express and
implied warranties, including but not limited to fitness for any other
purpose(s). In no event will Waters be liable for consequential, economic, or
incidental damages of any nature. Waters reserves the right not to honor this
warranty if the products are abused by the customer. The Warranty will not
be deemed to have failed of its essential purpose so long as Waters is able and
willing to repair or replace any nonconforming part or product.

Warranty service
Warranty service will be performed at no charge and at Waters’ option in one
of three ways:
• A service representative will be dispatched to the customer’s facility.
• The product will be repaired at a Waters repair facility.
• Replacement parts with appropriate installation instructions will be
sent to the customer.
Nonconforming products or parts will be repaired, replaced with new or
like-new parts, or refunded in the amount of the purchase price, when the
product is returned. Warranty service will be performed only if the customer
notified Waters during the applicable warranty period.
Unless otherwise agreed at the time of sale, warranty service will not be
provided by dispatching a service representative when the equipment has
been removed from the initial installation location to a new location outside
the home country of the selling company.

C-2 Warranty and Service Information


Warranty service exceptions
Warranty service will not be performed on:
• Any product or part which has been repaired by others, improperly
installed, altered, or damaged in any way.
• Products or parts identified before sale as not manufactured by Waters.
In such cases, the warranty of the original manufacturer will apply.
• Products that malfunction because the customer has failed to perform
maintenance, calibration checks, or observe good operating procedures.
Repair or replacement will not be made:
• For expendable items such as filament devices, panel lights, fuses,
batteries, and seals, if such items were operable at the time of initial use
• Because of decomposition due to chemical action
• For used equipment
• Because of poor facility, operating conditions, or utilities

Warranty period
The warranty period begins when the product is installed or, in the case of a
customer installation, 15 days after shipment from Waters.
In no case will the warranty period extend beyond 15 months from date of
shipment. If an item is replaced during its warranty period, the replacement
part will be warranted for the balance of the original warranty period.
The warranty period for the Waters Post-Column Reaction Module is as
follows:

1 Year Warranty Switches and Sensors


90 Day Warranty Cables
30 Day Warranty Replacement Parts and Service Workmanship
Expendable Items
a Ferrules, Compression Screws, Fuses, Tubing, and
Column Heater Inserts
a. Waters will replace only if shipped with manufacturing defects.

Limited product warranty C-3


Ordering information

Where to place orders


Write:
Waters Corporation
34 Maple St.
Milford, MA 01757
Attn: Order Processing Department
Call:*1-800-252-4752 - Customer Sales Department
Telex:174166 or 174128
Fax:1-508-872-1990
International Consult the listing of Waters Sales/Service offices at the end of
this manual.
Tip: Confirming orders mailed after a telephone order has been placed must
be clearly marked 'CONFIRMING' to avoid duplication.

How to place orders


Delays or errors in processing orders are frequently caused by incorrect or
incomplete information. To minimize delays and errors in processing your
orders, please list part numbers in ascending numerical order, and provide all
of the following information:
1. Catalog numbers and descriptions.
2. Quantity desired.
3. Complete purchase order number - orders cannot be processed without
it. Requisition numbers are insufficient.
4. Complete Ship To address and marking if applicable.
5. Complete Bill To address if other than Ship To.
6. Required delivery date.
7. Method of transportation desired.

C-4 Warranty and Service Information


8. Name and telephone number of person to contact if clarification is
required.

Part numbers
Appendix D, contains a list of the recommended replacement parts for the
Post-Column Reaction Module.

Pricing
Prices listed are FOB Milford, MA, unless otherwise agreed. Prices and
product information contained in any catalog or price list were current at the
time of printing. In a continuing effort to provide the finest products available,
Waters reserves the right to change specifications, models, or prices without
notice and without liability for such changes. Where price changes have
occurred, prices prevailing at time of receipt of your order will apply.

Payment terms
Our terms are net 30 days from invoice date with approved credit. If your
credit has not been previously established with Waters, our terms are
payment in advance or COD.

Shipments, damages, claims, and returns

Shipments
As all shipments are made FOB Milford, MA, we suggest insurance be
authorized on all shipments. Instruments and major components will be
packed and shipped via surface, unless otherwise required. Supplies and/or
replacement parts are packed and shipped via UPS, UPS Blue, air parcel post,
or parcel post unless otherwise requested.

Damages
The Interstate Commerce Commission has held that carriers are as
responsible for concealed damage as for visible damage in transit. Unpack
shipment promptly after receipt as there may be concealed damage even
though no evidence of it is apparent. When concealed damage is discovered,

Shipments, damages, claims, and returns C-5


cease further unpacking of the unit involved and request immediate
inspection by the local agent or carrier and secure a written report of his
findings to support claim. This request must be made within 15 days of
receipt. Otherwise, the claim will not be honored by the carrier. Do not return
damaged goods to the factory without first securing an inspection report and
contacting Waters for a return authorization number.

Claims
After a damage inspection report has been secured, Waters will cooperate
fully in supplying replacements and handling of a claim which may be
initiated by either party.

Returns
No returns may be made without prior notification and authorization. If for
any reason it is necessary to return material to us, please contact our
Customer Service Department or your nearest Waters
subsidiary/representative for a return authorization number and forwarding
instructions.

C-6 Warranty and Service Information


D RXN 1000 Coil Care and Use

Contents

Topic Page
Introduction D-2
RXN coil materials of construction/specifications D-2
Installation D-2
Helpful hints and precautions D-4
Ordering information D-5

D-1
Introduction
®
Waters RXN 1000 Reaction Coil is designed for liquid chromatography
applications where on-line chemical modification or derivatization of analytes
is required. The RXN Coil has several unique features which make it ideal for
post-column reaction systems:
• Inert fluid path compatible with most solvents and reagents, even at
elevated temperatures
• Proprietary knitted open tube design with minimal bandspreading to
maintain analytical resolution from high-performance columns

RXN coil materials of construction/specifications


• Volume: coil volume in µL is designated by descriptive number; e.g.,
RXN 1000 Coil has a volume of 1000 µL
• Coil: 0.018 inch ID polytetrafluoroethylene tubing knitted in a
proprietary manner
• Fittings: 1/16” compression screws and ferrules made of PEEK
• Jacket: anodized aluminum tube and endcaps
• Maximum Operating Temperature: 120 °C
• Maximum Operating Pressure: 500 psi (3.4 MPa)
• Tee: 316 SS, 90° port, low-dead volume design which accepts 1/16”
compression screw fittings

Installation
A typical post-column installation of the tee and RXN Coil is shown
schematically in the figure below.

D-2 RXN 1000 Coil Care and Use


One-stage post-column coil installation

From column
To detector
Dead-end fitting

Reagent

Tip: A second junction tee is present in the PCRM, but is not used for
applications that require a one-stage reaction.
A post-column installation for two reagents (using two tees) is shown
schematically in the figure below.

Two-stage post-column coil installation

From column
To detector
Reagent 2

Reagent 1

To install the post-column reactor:


1. Use 0.009-in. ID tubing for all sections of the fluid path through which
sample will flow. The reagent inlet line may be 0.020-in. ID or larger.
2. Thread the compression screw fittings into the appropriate tee or union
until finger tight. Do not overtighten.
3. Place the tee, RXN Coil, and associated tubing in the heating chamber.
This permits operation at a controlled temperature while also shielding
the coil and protecting it from damage.

Installation D-3
Helpful hints and precautions
• Support the coil so as not to place any strain on the exposed ends of the
PTFE tubing. Do not kink, stretch, scratch, or damage the exposed
PTFE tubing in any way.
• When installing the coil, do not overtighten the compression screws.
This can deform the ferrule, which, in turn, may place undue pressure
on the PTFE tubing and create a restriction in the fluid path leading to
excessively high system operating pressure.
• Filter reagent solutions before use with the Waters Solvent Clarification
Kit. Test a mixture of reagent solution and mobile phase beforehand to
make certain that precipitation will not occur in fluid path.
• Keep fluid moving through the coil while it is at temperatures above
ambient. Do not allow reagent solutions to sit in the coil at elevated
temperatures. Flush the RXN Coil clean immediately after use with a
suitable solvent.

Caution: If the exposed PTFE tubing at either end of the RXN


Coil becomes strained, compressed, or damaged in any way
and/or is subjected to internal pressure in excess of the
recommended maximum operating pressure, there is a risk that
mobile phase or reagent solution may leak in a high-velocity
stream from a small hole or break in the tubing. Always wear eye
protection, operate the coil in a closed chamber or behind a safety
shield, and shut off all fluid pumps, allowing sufficient time for
the internal pressure to be relieved, before inspecting, removing,
or servicing the coil.

D-4 RXN 1000 Coil Care and Use


Ordering information

Ordering information for the PCRM

Description Part number


RXN 1000 Coil Kit 030805
2.5 A Fuse WAT072919
SS Bulkhead Fitting WAT070216
SS Tee WAT075215
Thermal Switch 125 °C 700000978
CHEX Countercurrent Heat Exchanger 700000979
Reaction Coil Clamp 700000980
PEEK Tubing Kit, PCRM 700000984

To order by phone, call 800-252-4752 and then press 1 (U.S. and Canadian
customers only). To order by fax, dial 508-482-8449 (U.S.) or 905-678-2350
(Canada).
Send orders to:
Waters Corporation
Mail Stop: CS
34 Maple St.
Milford, MA 01757
Customers outside the U.S. or Canada, call your nearest Waters office.

Ordering information D-5


D-6 RXN 1000 Coil Care and Use
E System Startup Kit List

PCRM startup kit contents

Description/
Part number Quantity Item
Location
WAT021815 12 NM Compression Used to make
Screw 10-32 Short connections to LC
system
WAT021816 12 Compression Fitting Used to make
Knob connections to LC
system
WAT21817 12 NM PEEK Ferrule Used to make
1/16 inch OD connections to LC
system
WAT031795 1 PEEK Tubing Cutter Used to cut connection
tubings to LC system
WAT038051 1 Fuse Holder Fuse replacement
WAT038130 1 Fuse, 1.25A 250V Fuse replacement
WAT072919 1 Fuse, 2.5A Fuse replacement
WAT097559 1 Fuse Carrier 5 × 20mm Fuse replacement
289000511 1 Kit, Tubing, PCRM Used to make
Connections to LC
system
430000314 1 Tubing, Convoluted Connects drain outlet
to waste container
71500017204 1 Installation Guide, User installation and
Post Column Reaction operation information
Module

E-1
E-2 System Startup Kit List
Index
A I
audience and purpose v intended use v
ISM classification v
B
biohazard warning A-5 M
burst warning A-3 mass spectrometer shock hazard A-4
C O
caution symbol A-5 Ordering information C-4
Certificate of Validation 2-3
chemical hazard warning A-5 P
CHEX Countercurrent Heat Exchange Post-Column Reaction Module
Unit 1-3 voltage settings 2-4
Column heater Post-column reactor design 1-4
equilibrating 3-4 Powerup sequence 3-2
temperature limit, checking 3-4 Pump Control Module
temperature setting, checking 3-4 powerup sequence 3-2
turning off 3-3 purpose and audience v

D R
Damage Return information C-5
reporting 2-3 RXN Reaction Coil
Damage information C-5 care and use D-2
Data system hints and precautions D-4
powerup sequence 3-2 installation D-2

E S
EC Authorized Representative vi safety advisories A-1
electrical symbols A-12 Serial number 2-3
equipment guidelines iv, A-6 Shipping damage, reporting 2-3
Site selection 2-2
F Startup Kit 2-2
flammable solvents A-4 symbols
caution A-5
H electrical A-12
handling symbols A-13 handling A-13
Heater module, connections 2-4 warning A-2

Index-1
T
Temperature Control Module
erroneous entry, correcting 3-3
heater module, connections 2-4
powerup sequence 3-2
site selection 2-2
Temperature limit, checking 3-4
Temperature setting, checking 3-4
U
Unpacking 2-3
V
Voltage settings 2-4
W
warning symbols A-2, A-6
Warranty
period C-3
service C-2

Index-2

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