En Post Column Reaction Module
En Post Column Reaction Module
En Post Column Reaction Module
Reaction Module
Installation Guide
71500017204/Revision B
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.
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.
Applicable symbols
Symbol Definition
Manufacturer location
iv
Audience and purpose
This guide is intended for personnel who install the Waters Post-Column
Reaction Module.
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
v
residential locations and can be directly connected to a low voltage,
power-supply network.
EC authorized representative
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
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.
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.
~180° turns,
~90° out-of-plane
TP01710
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.
Electrical connections
Power switch
Temperature
control cable Fuse socket
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)
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.
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.
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.
This warning applies to certain instruments when they are in Operate mode.
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.
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.
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。
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。
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。
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。
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.
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。
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。
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。
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。
Electrical symbols
These can appear in instrument user manuals and on the instrument’s front
or rear panels.
Electrical power on
Standby
Direct current
Alternating current
Fuse
Keep upright!
Keep dry!
Fragile!
Use no hooks!
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.
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:
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
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,
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.
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
Installation
A typical post-column installation of the tee and RXN Coil is shown
schematically in the figure below.
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.
From column
To detector
Reagent 2
Reagent 1
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.
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.
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