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Varian

380-LC & 385-LC


ELS Detector

Operation Manual v1.1

Installation Category II
Pollution Degree 2
Safety Class 1 (EN 61010-1)

PL0890-0355
February 2008

Varian, Inc. offices


Varian ELS Detector

Varian, Inc. has offices in most countries. The major offices for
chromatography products are listed below:
Polymer Laboratories Ltd, now a part of Varian, Inc. (Manufacturing site)
Essex Road, Church Stretton,
Shropshire SY6 6AX, UK
International telephone: +44 1694 723581
International fax: + 44 1694 722171
Varian, Inc.
Scientific Instruments
2700 Mitchell Dr
Walnut Creek, CA 94598
Telephone: 1 800 926 3000
International telephone: +1.925.939.2400
International fax: +1.925.945.2360
Varian B.V.
Postbus 8005
4330 EA Middelburg, The Netherlands
International telephone: +31 118 67 1000
International fax: +31 118 62 3193
Varian Australia Pty. Ltd
679 Springvale Rd, Mulgrave,
Victoria 3170, Australia
International telephone: +61.3.9560.7133
International fax: +61.3.9560.7950
Varian Industria e Comercio Ltda.
Avenida Dr. Cardoso de Mello 1644
Sao Paulo 04548-005, Brazil
International telephone: +55.11.3238.0400
International fax: +55.11.3238.0410
Internet
The Varian, Inc. Internet home page can be found at:
www.varianinc.com
www.polymerlabs.com and www.varianinc.com
Polymer Laboratories, now a part of Varian, Inc., is the owner of copyright
on this document and any associated software. Under law, the written
permission of Varian, Inc. must be obtained before either the
documentation or the software is copied, reproduced, translated or
converted to electronic or other machine-readable form, in whole, or in
part.
First published February 2008 in Church Stretton, UK. Comments about this

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manual should be directed to the MarCom Manager, Polymer Laboratories,


Varian at the factory address above or by e-mail to:
marketing@polymerlabs.com
Polymer Laboratories, now a part of Varian, Inc. is ISO9001:2000 certified.
€ 2008 Polymer Laboratories, now a part of Varian, Inc.
Varian, the Varian Logo and Galaxie are trademarks or registered
trademarks of Varian, Inc. in the U.S. and other countries.
• All product and company names herein may be the trademarks of their
respective owners.
All rights reserved.

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Varian ELS Detector

Contents

Safety Practices and Hazards .......................................................... 8


General 8
Electrical Hazards 9
Hot Surface Hazards 10
High Pressure Hazards 10
Cleaning 11
Other Precautions 11
Warning and Caution Messages 12
Warning Symbols 13
CE Compliance 14
Local Varian Offices or Distributors 14
1. General Information ............................................................... 15
1.1 Introduction 15
1.2 Pre-installation Requirements 15
1.3 User Documentation 15
1.3.1 Conventions 16
1.3.2 Notes and hot tips 16
1.4 Specifications 16
1.5 Unpacking and Installation 18
1.6 Packing List 18
1.7 Site Preparation Checklist 19
1.8 Location of the Detector Module 20
1.9 Do’s and Don’ts of ELS Detection 20

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1.9.1 Pumping systems 20


1.9.2 Mobile phase priming 21
1.9.3 Solvent recommendations 21
2. Installation.............................................................................. 22
2.1 Installation Checklist 22
2.2 Power Connections 23
2.3 Extraction 23
2.4 Gas Connection 23
2.5 Other Connections 24
2.5.1 Digital output 26
2.5.2 Analogue output 26
2.5.3 Connection to a Varian Star 800 Module Interface Box 26
2.5.4 Control I/O connector 26
2.6 Fluid Connection 27
2.6.1 Inlet 27
2.6.2 Outlet 27
2.7 Connecting the Detector to your LC System 28
2.8 Connecting the Detector to your PC 29
2.9 Varian ELS Detector Software Control 30
2.10 Installing the Standalone Software Utilities 30
2.10.1 Configuring the Software Utilities 31
2.11 Installing the Galaxie Driver Software 31
2.11.1 Reinstalling or upgrading the Galaxie driver 33
2.11.2 Configuring the Varian ELS Detector in Galaxie 33
2.12 Installing the ELSD driver for ChemStation• 34
3. System Description and General Operation .......................... 35
3.1 Basic Principles of Operation 35
3.1.1 Theory 36
3.2 Operational Parameters 37
3.3 Instrument Controls 38
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3.3.1 Display Screen 38


3.3.2 Keypad 39
3.3.3 Main menu bar 39
3.3.4 Sub- Menu Screen 40
3.3.5 Status Mode 40
3.3.5.1 Standby 41
3.3.5.2 Run 41
3.3.6 Error conditions 41
3.3.7 Clearing an Error 42
3.4 Operational Parameters 42
3.4.1 Method 42
3.4.1.1 Loading a Method 42
3.4.2 Evaporator Temperature 43
3.4.3 Nebuliser Temperature 44
3.4.4 Evaporator Gas Flow 44
3.4.5 Detector Gain (PMT) 44
3.4.6 Response Time (Smoothing) 45
3.4.7 Light Source Intensity (LED) 45
3.4.8 Power Mode 45
3.4.9 Data Output Rate (Hz) 46
3.5 Controlling the Varian ELSD Using the Standalone Software Utilities46
3.5.1 Control Software-Overview 46
3.5.2 Control Software-Parameter Settings 47
3.5.3 Control Software-System Test 48
3.5.4 Method Editor Software-Overview 48
3.5.5 Method Editor-Creating & Storing Methods 49
3.5.6 Method Editor-Downloading Method Sets 49
3.6 Controlling the Varian ELSD During an Injection 50
3.6.1 Real-time operation 50
3.6.2 Creating a real-time program 50

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3.6.3 Starting & stopping real-time control 50


3.7 Controlling the Varian ELSD Using Galaxie 51
3.7.1 Galaxie Status window 52
3.7.2 Galaxie Connection status 53
3.7.3 Galaxie Status Overview 54
3.7.4 Automating the Varian ELS Detector 54
3.8 Controlling the Varian ELSD within ChemStation• 55
3.9 General Considerations 56
3.9.1 Solvent recommendations 56
3.9.2 Sample preparation 57
3.9.3 Column Considerations 58
3.9.4 Transferring ELSD Methods 58
4. Routine Maintenance ............................................................. 59
4.1 Drying the Diffuser 59
4.2 Cleaning Evaporator Tube 60
4.3 Information for Service Personnel 60
4.3.1 Heater PCB Fuses 60
4.3.2 Light Source 61
4.4 Putting the Instrument into Storage 61
4.5 Upgrading the Firmware 61
4.5.1 Tools required 61
4.5.2 Firmware upgrade procedure 62
5. Troubleshooting ...................................................................... 63
5.1 Troubleshooting an HPLC System 63
5.2 Instrument Errors 64
5.3 General Problems 65
APPENDIX 1 – Method Record ...................................................... 68
APPENDIX 2 – Spare Parts Listing .................................................... 69
APPENDIX 3 – Cleaning and Decontamination Procedure ................ 70

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Varian ELS Detector

Safety Practices and Hazards

Your Varian instrument and accessories have been carefully designed so


that when used properly you have an accurate, fast, flexible and safe
analytical system.
Information about safety practices appears throughout the documentation
(both hard copy and online) provided with your instrument and accessories.
Before using the instrument or accessories, you must thoroughly read
these safety practices.
Observe all relevant safety practices at all times.
This instrument is designed for chromatographic analysis of appropriately
prepared samples. It must be operated using appropriate gases and/or
solvents and within specified maximum ranges for pressure, flows, and
temperatures as described in this manual. If the equipment is used in a
manner not specified by the manufacturer, the protection provided by the
equipment may be impaired. Varian assumes no liability for the customer’s
failure to comply with these requirements.
It is the responsibility of the customer to inform Varian Customer Support
Representatives if the instrument has been used for the analysis of
hazardous biological, radioactive, or toxic samples, prior to any instrument
service being performed or when an instrument is being returned to the
service center for repair.

General
Operation of a Varian ELS Detector involves the use of pressurized liquid
and hazardous materials including corrosive fluids and flammable liquids.
Careless, improper or unskilled use of this ELS Detector can cause death or
serious injury to personnel, and/or severe damage to equipment and
property.
The Varian ELSD incorporates covers that are designed to prevent
inadvertent contact with any potential hazards. If the instrument is used in
any manner not specified by Varian, this protection may be impaired. It is
essential that no cover is bypassed, damaged or removed.
The safety practices described below are provided to help the user operate
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the instrument safely. Read each safety topic thoroughly before attempting
to operate the instrument and ALWAYS operate the ELS Detector in
accordance with these safety practices.
Follow these safety practices to ensure safe equipment operation.
 Perform periodic leak checks on all supply lines and pneumatic
plumbing.
 Do not allow gas lines to become kinked or punctured. Place lines
away from foot traffic and extreme heat or cold.
 Store organic solvents in fireproof, vented and clearly labeled cabinets
so they are easily identified as toxic and/or flammable materials.
 Do not accumulate waste solvents. Dispose of such materials through
a regulated disposal program and not through municipal sewage lines.
This instrument has been tested per applicable requirements of LVD & EMC
Directive as required to carry the European Union CE Mark. This equipment
may be susceptible to radiation/interference levels or frequencies that are
not within the tested limits.

Electrical Hazards
Exposure to high voltages can cause severe skin damage and cataracts of
the eyes, while close contact with the electrical components can result in
severe heat burns to the skin, and an electrical discharge which may cause
death, severe electric shock or sub-surface skin burns.
The ELS Detector has been carefully designed to operate safely and
effectively when using components that conform to Varian’s design
criteria. Use of non-approved components in the detector may render the
system inoperative and/or hazardous. It may also invalidate the warranty
on the instrument. Use only related components supplied or authorized by
Varian.
Voltages above 110 V AC are present within the instrument.
 Disconnect the instrument from all power sources before removing
protective panels to avoid exposure to potentially dangerous voltages.
ONLY Varian-trained, Varian-qualified, or Varian-approved Customer
Service Representatives may open panels or covers that are retained
by screws on the detector. Consult the manuals or product labels
supplied with your instrument to determine which parts are operator-
accessible.
 Whenever it is likely that the protection has been impaired, the
instrument must be made inoperative and be secured against any
unintended operation.
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Varian ELS Detector

 When it is necessary to use a non-original power cord plug, make sure


the replacement cord adheres to the color-coding and polarity
described in the manual and all local building safety codes.
 Good grounding/earthing is essential to avoid a potentially serious
electric shock hazard. Consult the manuals or product labels supplied
with your instrument for the relevant grounding requirements.
 Replace blown fuses with fuses of the size and rating shown on the
fuse panel or in the manual.
 Replace faulty or frayed power cords immediately with the same type
and rating.
 Ensure the power switch and appliance coupler at the rear of the
instrument remain easily accessible at all times.
 Make sure that voltage sources and line voltage match the value for
which the instrument is wired.
 Avoid using power supplies from a source that may be subject to
electrical or RF interference from other services (for example, large
electrical motors, elevators and welders).
 This instrument contains a light source, which has been classified
according to the methods specified in IEC 60825-1 Ed 1.2 as a CLASS
1 LED PRODUCT.

Hot Surface Hazards


Hot surfaces may be exposed when the instrument is opened. These are
indicated by a warning label. Allow these surfaces to cool before touching
them.

High Pressure Hazards


If a solvent line ruptures, a relief device opens, or a valve opens
accidentally under pressure, potentially hazardous high liquid pressures can
be generated by the pump causing a high velocity stream of volatile and/or
toxic liquids.
 Wear face protection when you inject samples or perform routine
maintenance.
 Never open a solvent line or valve under pressure. Stop the pump first
and let the pressure drop to zero.
 Use shatterproof solvent reservoirs capable of operating at 50/60 psi.
 Keep the solvent reservoir enclosure closed when the reservoir is

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under pressure.
 Read and adhere to all NOTES, CAUTIONS, and WARNINGS in the
manual.

Cleaning
The individual or group responsible for the use and maintenance of this
equipment must ensure that appropriate decontamination is carried out if
hazardous material is spilt on or inside the instrument.
Before using any cleaning or decontamination method except those
recommended by Varian, users should check with Varian that the proposed
method will not damage the equipment.
See Appendix 4 for detailed recommended procedures.

Other Precautions
Use of the ELS detector and accessories may involve materials, solvents
and solutions that are flammable, corrosive, toxic or otherwise hazardous.
Careless, improper or unskilled use of such materials, solvents and
solutions can create explosion hazards, fire hazards, toxicity and other
hazards that can result in death, serious personal injury or damage to
equipment.
Always ensure that laboratory safety practices governing the use, handling
and disposal of hazardous materials are strictly observed. These safety
practices should include wearing appropriate safety clothing and safety
glasses.
Airflow to the cooling fans of the ELS detector and accessories must be
unobstructed. Do not block the ventilation grills on the detector and
accessories. Consult the manuals supplied with your PC and monitor for
their specific ventilation requirements.
Keep solvents from direct contact with polyurethane gas supply tubing, as
certain solvents will cause weakening and leaks with possible bursting.
All components of the system should be connected to a common power
supply and common ground. This ground must be a true ground rather than
a floating ground.
Eluents containing non-volatile mineral acids or bases should be avoided
Employ static measuring and static discharge devices (e.g., air ionizers) to
safeguard against the buildup of static electricity.
The unit should not be stacked more than two high without additional
means of support and suitable precautions should be taken to prevent the
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Varian ELS Detector

units being knocked over.


The detector weighs approximately 11.0 kg (24.2 lb). To avoid injury to
personnel or damage to the instrument or property, always use suitable
lifting procedures to move the instrument.
Use only Varian-supplied spares with your instrument.

Warning and Caution Messages


A Warning message is used in the text when failure to observe instructions
or precautions could result in death or injury. The list of symbols that
appear in conjunction with warnings are detailed in the next section.
A Caution message is used when failure to observe instructions could
result in damage to equipment (Varian supplied and/or other associated
equipment).

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Warning Symbols
The following is a list of symbols that appear in conjunction with warnings
in this manual or on the ELS Detector. The hazard they describe is also
shown.
A triangular symbol indicates a warning. The meanings of the symbols that
may appear alongside warnings in the documentation or on the instrument
itself are as follows:

Corrosive liquid Electrical shock Explosion hazard

Eye hazard Fire hazard Heavy weight


(danger to feet)

Heavy weight Hot surface Moving parts


(danger to hands)
The following symbol may be used on warning labels attached to the
instrument. When you see this symbol, refer to the relevant operation or
service manual for the correct procedure referred to by that warning label.

The following symbols appear on the instrument for your information.

I Mains power on.

0 Mains power off.

Fuse.

Single phase alternating current.

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Direct current.

When attached to the rear of the instrument, indicates


that the product complies with the requirements of
one or more EU directives.

When attached to the rear of the product, indicates


that the product has been certified (evaluated) to CSA
1010.1 and UL 3101-1.

CE Compliance
Your Varian ELS Detector has been designed to comply with the
requirements of the Electromagnetic Compatibility (EMC) Directive and the
Low Voltage (electrical safety) Directive (commonly referred to as the LVD)
of the European Union. Varian has confirmed that each product complies
with the relevant Directives by testing a prototype against the prescribed
EN (European Norm) standards.
Proof that a product complies with these directives is indicated by:
 the CE Marking appearing on the rear of the product, and
 the documentation package that accompanies the product containing a
copy of the Declaration of Conformity. The Declaration of Conformity is
the legal declaration by Varian that the product complies with the
directives listed above, and shows the EN standards to which the
product was tested to demonstrate compliance. It is also signed by
Varian Authorized Representative in the EU, and by the representative
of the manufacturing plant.

Local Varian Offices or Distributors


We stress the importance of standard laboratory safe practice (e.g., COSHH
regulations) for dealing with electronic laboratory equipment, solvents,
etc., in preventing accidents, fires, or potentially hazardous conditions.
If in any doubt about the use of the instrument contact your local Varian
office or local distributor.
The Varian, Inc. Internet home page can be found at:
www.varianinc.com

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1. General Information

1.1 Introduction
The Varian 380-LC & 385-LC Evaporative Light-Scattering Detector (ELSD)
is a unique and highly sensitive detector for semi-volatile and non-volatile
solutes in a liquid stream. It is mainly used as a concentration detector for
High Performance Liquid Chromatography (HPLC). The solvent stream
containing the solute material is nebulized and carried by a gas flow
through an evaporation chamber. The solvent is volatilized, leaving a mist
of solute particles that scatter light to a photosensitive device. The signal
is amplified and a voltage output provides the concentration of the solute
particles passing through the light.
The Varian ELS Detector may be used alone, or as one of several detectors
in a GPC or HPLC system. As the solvent or eluent is evaporated in the
course of the analysis, the ELSD must be the last in series if used in
conjunction with other detectors. If the ELS detector is being used as the
last detector in a series, care must be taken not to exceed the
recommended backpressure in detector cells in other units.
This manual instructs the user in the installation and operation of the
Varian ELS detector for stand-alone and Galaxie Chromatography software
control.

1.2 Pre-installation Requirements


The Varian ELS Detector operation manual describes the environmental and
operating requirements of the ELSD. You must prepare your laboratory
according to these instructions before the detector can be installed. If you
have misplaced your copy, you can obtain a replacement from your local
Varian office. Alternatively, download a PDF from the Varian, Inc. Web site,
www.varianinc.com

1.3 User Documentation


You have been provided with this operation manual to help you set up and
operate your ELS detector. This operation manual contains safety practices
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and hazards information, where to find information about installing and


maintaining instrument components and a brief operation overview.

1.3.1 Conventions
The following conventions have been used throughout the documentation:
 Menus, menu options and field names (e.g., choose Copy from the Edit
menu) have been typed in bold. Bold is also used to signify the buttons
appearing throughout the software (e.g., click OK).
 ALL CAPITALS indicate keyboard commands (e.g., press the F2 key) and
text you must type in from the keyboard (e.g., type SETUP at the
prompt).

1.3.2 Notes and hot tips


A Note is used to give advice or information. A Note is denoted by the
following symbol: 2.
A Hot Tip is used to give practical hints to help you achieve the best
possible performance from your instrument. A Hot Tip is denoted by the
following symbol: PPP.

1.4 Specifications
The instrument is suitable for indoor use only and is classified suitable
under the following categories (EN 61010-1):
Installation category II
Pollution degree 2
Safety class 1

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Light Source LED 480nm (Class 1 LED product)


Detector PMT with digital signal processing
Nebuliser OFF, 30-90 ƒC
Evaporator
Varian 380-LC OFF, 25-120 ƒC
Varian 385-LC 10-80 ƒC
Gas Flow Range 0.9-3.25 SLM with controlled gas shut-off valve
Operating Pressure 60-100 psi (4-6.7 bar)
Eluent Flow range 0.2-5.0 mL/min
Digital Output 10 or 40Hz (24bit)
Analogue Output 0-1V FSD
Serial (RS232)
Communication Remote Start Input
Pump Stop: 1 Contact closure
Power Requirements 90/120V AC or 220/250V AC 50/60 Hz 2A Max
Power consumption 150 W (max)
Dimensions (wxdxh) (unpacked) 200 x 450 x 415 mm
Weight (unpacked) 11 kg (380-LC) 13 kg (385-LC)
Weight (packed) 16 kg (380-LC) 18 kg (385-LC)
Galaxie Chromatography Software
Varian ELSD Control Software
PC control (software) Varian ELSD Dimension Software
Varian ELSD driver for ChemStation•
Chromeleon• CDS
Remote operation Remote Start Input
Safety features Gas shut off Valve, Leak Detection

Table 1. Performance Specification of the Varian ELS Detector

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1.5 Unpacking and Installation


Care has been taken to ensure that the instrument should be received in
proper condition. The packing and protection are designed for normal
hazards of road, rail or air transit. Any damage to the container or
instrument should be reported immediately to your local distributor, or to
Varian. It is recommended that the shipping container be kept, if possible,
for re-shipment or return to a service centre.
Examine the shipping carton for visible signs of exterior damage. Unpack
the instrument and examine it for transit damage. Check that all items on
the packing list are included.
Notify your local distributor or Varian of any damage or missing items.

1.6 Packing List


 Varian ELS Detector
 Operation Manual[SMB1]
 ELSD Control Software[SMB2]
 Mains leads (UK, EUR, USA)
 RS232 data cable
 Analogue output Cable
 Gas Tubing (2 m)
 PVC Exhaust hose (2 m)
 Tygon• SE200 waste hose (7 cm)
 500 mL Solvent waste container

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1.7 Site Preparation Checklist

Environmental conditions Temperature 10 to 35 €C (50 to 95 €F).


At constant temperature.
Avoid positioning in direct sunlight.
Humidity 10-80%.
Power USA & Japan 115V (AC) •10%.
50/60 Hz, 2A max, with protective earth connection.
Europe 230V (AC) •10%.
50/60 Hz, 2A max, with protective earth connection.
Note: Ensure the power switch and appliance coupler
remain accessible at all times.
Bench space The standard instrument will require the following bench
space:
 width 25 cm (9.8”)
 depth 60 cm (23.6”)
 height 41.5 cm (16.3”)
Note: The instrument can be computer controlled and
additional bench space will be required for the computer.
Gas Supply Nitrogen (>98% purity, filtered to 0.2 ‚m).
Air can only be used for non-flammable solvents.
The instrument is not calibrated for use gases other than
Air or Nitrogen.
For operation with other inert gases contact Polymer
Laboratories Varian for advice.
Extraction requirements The exhaust gases from the instrument must be extracted
to a fume cupboard or similar extraction unit.
The PVC extraction tube provided can be extended if
necessary, provided the diameter of the extension tube
used is >50 mm.

Table 2. Site preparation checklist

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Warning
The ELS Detector weighs approximately 11.0 kg (24.2 lb). To avoid injury
to personnel or damage to equipment, always follow all precautions for
lifting heavy objects when moving the instrument. It is advisable to
locate the system on a sturdy bench.

1.8 Location of the Detector Module


Place the detector conveniently near your HPLC system. The modular
design of the Varian ELSD enables you to locate it anywhere within the
limitations imposed by the length of the power cord, fluid lines and signal
cables.
In order to keep liquid dead volume as low as possible and to minimize
peak broadening in the lines, the distance between the column outlet and
the flow cell inlet should be kept to a minimum.
Provide approximately four inches of space behind the unit so that the
cooling fan intake is not impeded, and to allow easy access to the rear
panel.
The ELS detector can be placed within 2 meters of an extraction unit, using
the exhaust tube provided.

1.9 Do’s and Don’ts of ELS Detection


1. NEVER block the exhaust outlet as this causes increased
back-pressure on the nebulisation chamber. High pressures on the
internal chamber will lead to increased baseline noise and low
sensitivity.
2. NEVER allow the solvent waste outlet tube to become immersed
in the waste solvent as this will create backpressure on the
nebulisation chamber; leading to increased noise.
3. When placing more than one HPLC detector in series, always
place the ELS detector last.
4. Only volatile mobile phase additives can be used the ELSD. See
Table 6 (pg 57). The use of non-volatile buffers will lead to
increased baseline noise levels.

1.9.1 Pumping systems


It is recommended to use a high-performance pumping system (e.g. 920-
LC) with no flow pulses to minimize nebulisation problems. Inconsistent
solvent flow will result in poor reproducibility.

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A backpressure regulator maybe necessary on certain pumps in order to


minimize pulsation. This can also be achieved by the column itself or a coil
of 0.005” ID tubing placed between the pump and the column.
If pulse damping is needed, use the Varian Pulse Reduction Accessory (Part
No. 0391970101) or the Ultra High Pulse Reduction Accessory (Part No.
0391970102).
For the Varian 900-LC series, no special operating pressure is required.

1.9.2 Mobile phase priming


The Varian ELS detector does not require any mobile phase priming, other
than that required to prime the solvent through the pump, damper,
injector, column, etc. It is recommended that priming of the LC system be
performed without the ELS detector attached, to prevent non-volatile
impurities contaminating the ELS detector.
The mobile phase should be degassed and filtered, either by sparging with
Helium or using an on-line degasser (Part No. A6313).

1.9.3 Solvent recommendations


The maximum operating temperature of the detector and the boiling point
of the solvent will determine the type of solvents compatible with the
Varian ELS detector. High boiling point solvents such as
N-methylpyrrolidinone (NMP), Dimethylsulphoxide(DMSO),
Dimethylacetamide (DMac), m-Cresol and 1,2,4, Trichlorobenzne (TCB) are
not recommended for long-term operation. Greater care and attention to
instrument cleaning procedures should be exercised with these solvents.
It is recommended that any solvent be flushed from the detector for
overnight and weekend storage.

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Varian ELS Detector

2. Installation

The Varian ELS Detector must be installed by a Varian-trained, Varian-


qualified or Varian-authorized customer support representative.
Details for unpacking the instrument and what to do in case it has been
damaged in transit are outlined in this operation manual in Chapter 1,
Section 1.5.
This chapter describes how to install the ELS detector.

2.1 Installation Checklist


Your CSR will:
 Unpack the Varian ELSD.
 Remove all packing list items that are shipped with the instrument
(including this operation manual) and present them to you for review.
 Unpack the accessories supplied with the instrument and check that
you have received everything on the packing lists (enclosed in the
packing crate and inside each accessory box).
 Install your ELS detector.
Although the Varian-trained, Varian-qualified or Varian-authorized
customer support representative will install the hardware and any
necessary Galaxie driver software for you, you may need to install
hardware or software yourself at some later stage, for example if you move
the ELS detector or change the PC.
To install the ELS detector:
 Connect the power and communication cables.
 Connect the gas & solvent outlet tubing.
 Connect the solvent inlet tubing to the detector.
 Install the ELSD software driver on the PC.
 Configure the ELSD software driver.

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2.2 Power Connections


Before connecting the power cable, ensure the instrument voltage rating
matches your local power supply.
 Use only a supply with protective grounding.
 The correct fuses should be installed.
 For 115V (AC) or 230V (AC) use two 250V H 2A T 20 x 5 mm fuses.
2 Note This unit is double-fused.

Warning
Risk of fire, replace fuses as marked.

2.3 Extraction
The ELS detector is provided with tubing for venting the exhaust gases and
vapors, and so does not need to be placed in a fume cupboard. Instead, the
exhaust hose provided must be attached to the rear of the unit and vented
to a fume hood or other disposal unit. Ensure the exhaust hose has an
upward slope from the detector so that any condensed solvent is collected
in the waste bottle at the front of the unit and to prevent it accumulating
in the tubing.
2 Note The exhaust must be extracted to a suitable fume extraction system.

2.4 Gas Connection


The instrument should be supplied with clean, dry nitrogen gas between
60-100 psi in pressure. For optimum performance a gas pressure of 60 psi
is recommended. A convenient 4 mm push-in connection for the gas
source is provided at the rear of the instrument.
To prevent against unnecessary gas usage, a controlled gas shut off valve is
integrated into the detector gas manifold. This will only allow gas to pass
into the instrument when in RUN mode. Should the instrument default to
STANDBY mode the gas will reduce to a default value of 1.2 SLM for 15
mins before closing.

Caution The gas inlet valve will be closed when the instrument is first powered
on in STANDBY and will only open once the instrument is set to RUN
mode.

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Varian ELS Detector

2.5 Other Connections


All power, signal and communication connections are made on the rear
panel of the ELS detector, see Figure 2. The connectors on the rear of the
panel support communication configurations to a range of devices, such as
autosampler, pumps, valves and injectors.

Figure 1. Front view of the Varian ELS Detector


1. Front screen display
2. Keypad
3. Eluent inlet
4. Solvent waste outlet

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Varian ELS Detector

11
2

3
10 4

9 6

7
8

Figure 2. Rear view of the Varian ELS Detector


1. External Vapor Sensor 6. Mains Switch
2. Serial RS232 connector-24bit digital 7. Mains Input
output
8. Fuses
3. Service Connector
9. Gas supply inlet port
4. Service Switch (run/flash)
10. Exhaust port
5. Remote Start Input
11. Analogue Output (1V

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Varian ELS Detector

2.5.1 Digital output


The Varian ELS Detector is fitted with a standard RS232 (DTE-DCE) 3-wire
serial interface.
The serial RS232 connector provides a 24bit (10 or 40Hz) digital output for
connection to a PC running a data acquisition package (e.g. Galaxie
Chromatography software). For further information on how to configure
the PC for with Galaxie software see Section 2.11 (pg 31).
If controlling the instrument from a PC, a free serial port is required. A USB
port on the PC can be used but a USB-to-Serial adapter is required (Part
No. PL0860-0620).
The Varian ELS detector is also fitted with a service connector, located
below the RS232 port, for flash upgrading firmware (see Figure 2).

2.5.2 Analogue output


The Varian ELS Detector is supplied with a 1V analogue output cable (Part
No. PL0890-0300) that allows data collection via an A/D interface, such as
a Star MIB 800 module. The gold end fitting of the analogue cable plugs
into the gold pin on the rear of the detector and the opposite end connects
to the positive and negative inputs of the A/D interface.

2.5.3 Connection to a Varian Star 800 Module Interface Box


The Star 800 Module Interface Box (MIB) provides analogue-to-digital
signal conversion (ADC). Connections are made by connecting the analogue
output cable to one of the analogue signal input ports on the middle right
side of the Star 800 MIB. For more information about connecting your
Varian ELS Detector to a Star 800 MIB, refer to your Star 800 MIB
documentation.

2.5.4 Control I/O connector


The Varian ELS Detector can be connected to auxiliary equipment, such as
an autosampler, or pump via the 15pin I/O connector. The I/O connector
can be configured in several ways to allow on-board timetable events to be
triggered or to remotely auto-zero and shutdown the detector.
The ELS detector is equipped with 2 contact closures (normally-open) for
stopping the operation of a pump if the unit reports an error condition.
The Varian ELS Detector is also equipped with one contact closure, which is
normally open, and two TTL logic inputs, both active-low (with internal
pull-up resistors to 5 V).
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Varian ELS Detector

Note Pump stop facility must be employed if the instrument is to be left


unattended, or if units are stacked.

I/O description Pin number


Inputs Remote Start 14 & ground
Remote Standby 13 & ground
Remote A/Z 7 & ground
Output Pump stop contact closure – normally open 3 & 10
Ground (to case) 1, 5, 6, 11

Table 3. Varian ELS Detector I/O connections


In order to make appropriate remote standby and A/Z connections for the
I/O socket, an I/O cable can be purchased from Varian, Inc. (Part No.
PL0890-0345). For remote start operation, a specific cable is required that
can be purchased from Varian, Inc. (Part No. PL0890-0350).

2.6 Fluid Connection

2.6.1 Inlet
The eluent from the chromatography system is connected to the central
front port of the Varian ELS Detector via a low dead volume Valco•
bulkhead connector.
The liquid inlet port is connected directly to the nebuliser by a short length
(130 mm) of capillary tube giving a delay volume from port to nebuliser tip
of ~4 †L.

2.6.2 Outlet
The waste eluent is expelled from the detector via the front outlet tube.
The outlet tube should be connected to the 500 mL waste bottle using the
supplied Tygon• tubing of 40 mm ID.
For long periods of use, it is recommended that a larger solvent container
be used to prevent the solvent overflowing.

Caution Check all connection carefully for leaks before replacing the front panel.

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Varian ELS Detector

Warning
Do not allow the solvent waste tube to be submersed below the
solvent level inside the container. This will cause positive pressure to
be exerted on the nebuliser chamber causing excessive baseline noise.

2.7 Connecting the Detector to your LC System


To connect the detector:
1. Connect the power cord to the IEC inlet at the rear of the unit.
2. Check the operating voltage of your instrument, 110V 2A or 230V
2A, on the IEC inlet fuse-holder on rear of unit.
3. Attach the 4 mm OD gas tube into the gas inlet port at the rear of
the instrument (see Figure 2). The gas connection is a push-in
fitting.
4. The gas should be dry, filtered and have a minimum inlet pressure
of 60 psi, 60-100 psi is required to achieve the maximum
operating instrument gas flow rate of 3.25 SLM.
5. Connect the solvent waste tube to the waste outlet at the front
of the detector and position the other end into a waste collection
bottle.
6. The solvent waste container supplied with the detector can be
sited on the bench in front of the instrument. Alternative waste
collection vessels can be used if required but the bottom of the
waste tube must be below the height of the waste outlet from
the instrument. Waste tube must NOT be submerged in the liquid.
7. Connect the exhaust hose between the exhaust outlet and a fume
hood.
8. For analogue data collection, connect the instrument to an A/D
module (e.g. MIB 800) using the analogue cable provided.
9. For digital data collection using Galaxie Software, connect the
instrument, using the RS232 communication cable, between the
detector’s rear serial port and PC. The PC must have a free serial
port.
10. Connect the LC column outlet to the eluent inlet at the front of
the unit) using the shortest length of tubing possible (1/16” OD,
0.010” ID).
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Varian ELS Detector

11. Turn on the source gas to a pressure of about 60-100 psi.


12. Switch on the Varian ELS Detector, and select a desired method
(e.g. Method “XXX”).
13. Initiate heating by selecting RUN mode using the arrow keys on
the front keypad.
14. When the unit has reached temperature, the baseline noise
should be checked to ensure that it is < 0.2mV peak-peak. This
verifies that the gas supply is clean and dry.
15. If the baseline is within the limits, Autozero the detector.
16. Turn on the eluent flow and allow the system to stabilize.
17. Again check the baseline noise. It should not have increased
significantly and should be 0.5mV. Typically pure water should
give no more than 0.4mV peak-peak, whilst pure organic solvents
should be less than 0.3mV.
If the baseline noise is excessive, then please refer to the
troubleshooting Section in Chapter 5. Where noise and all other
conditions are acceptable, the instrument is ready to begin work.
Note: Some volatile buffers can generate considerable offsets and increased
noise levels.

2.8 Connecting the Detector to your PC


To operate the Varian ELS Detector with any software package a free Serial
(RS-232) communications port (1 to 255) is required on your PC. Most
computers are supplied with at least one serial port as standard, but if your
PC does not provide a serial port or you are already using the existing serial
ports for other devices, then there are a couple of options available to you:
1. Use a Universal Serial Bus Interface (USB)
If your PC has one or more Universal Serial Bus (USB) connectors then you
can use a “USB – Serial Port Adaptor” (Part No. 0860-0620), which
provides a Serial Port connection to your PC. The Universal Serial Bus
interface is supported on:
Windows 98
Windows ME
Windows 2000
Windows XP

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Varian ELS Detector

Note: USB is NOT Supported on NT 4.0. You may require extra software to use
USB on Windows.

2. Adding an Extra Serial Card to your PC - Using Multiple Serial Ports


Multiple Port Serial cards are available, which allow 4, 8 and 16 extra serial
ports to be added to your PC using a single PCI card.
Ensure that the Varian ELS Detector is switched on and operating normally.
Make sure you have one free and valid RS-232 communications port (1 to
255).
Connect a serial port on your PC to the port labeled "RS232" on the rear of
the detector. Ensure that the service switch, (see Figure 2, pg 25) is
located in the RUN position (i.e. Upwards).

2.9 Varian ELS Detector Software Control


The Varian ELS Detector comes supplied with standalone software utilities
for basic instrument control. An optional additional software package
called DIMENSION that programs the detector for real-time control during
an injection is available from Varian (Part No. PL0890-0375).
The Varian ELS Detector is also controllable via Galaxie Chromatography
Software, with the added advantage of digital data acquisition via serial
communication. The Galaxie control software for the ELSD can be
purchased from Varian Inc (Part No. 8510244000).
A software driver to allow control of the Varian ELSD through
ChemStation• is available from Varian, Inc. (Part No. PL0890-0380).

2.10 Installing the Standalone Software Utilities


Two software utilities are provided with your Varian ELSD, namely Control
and Method Editing software.
To install the software utilities, you must have administrator rights for the
PC. When you insert the supplied software CD into your CD drive, the CD
browser will start automatically. If it does not, you can launch the browser
by running Setup.exe from the root directory of the CD.
Note: The Standalone Software utilities are only compatible with Windows 2000 & XP
Pro.

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Varian ELS Detector

2.10.1 Configuring the Software Utilities


On starting the ELSD Control Software or Method Editor program, the
correct Serial Port must be configured for successful communications. The
ELSD software needs to be configured for the Serial Port you are using on
your PC.
The first time the ELSD Control Software is used, the detector will be
allocated to Serial Port COM 1.
As various control packages for the detector use the same port on the
detector you must terminate the Control software before starting Galaxie
or ChemStation • software, and vice versa.
For information on how to operate the Control & Method Editor software,
please refer to Section “Controlling the Varian ELSD Using the Standalone
Software Utilities” (pg 46).

2.11 Installing the Galaxie Driver Software


The Varian ELSD Galaxie Driver software is installed as part of the Varian
LC driver’s package (Part No. 8510244000). Before installation, check that
the ELSD firmware is compatible with the Galaxie software control.
To install the Varian LC drivers, Galaxie software must already be installed
and you must have administrator rights for the PC.
The Varian drivers must be installed only on the server.
When you insert the Galaxie CD into your CD drive, the CD browser will
start automatically. If it does not, you can launch the browser by running
Install.exe from the root directory of the CD.
From the CD browser, click on the Install Varian Drivers button.
Then click on the Install Varian LC button.
The following screen will appear:

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Varian ELS Detector

Click on the Next button, read and accept the License Agreement and
enter your driver Serial Number corresponding field. The serial number is
provided on your driver serial number card and is different from the Galaxie
serial number.

Note: The serial number is case sensitive.

Then press the Next button and click on Finish at the end of the
installation.

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Varian ELS Detector

2.11.1 Reinstalling or upgrading the Galaxie driver


If you want to reinstall or upgrade your drivers, you will need to run the
setup again, until the following screen appears:

Press Next and the drivers will be automatically reinstalled or upgraded.


Click on Finish at the end of the installation to exit the maintenance mode.
To see which drivers are installed, select Options from the Galaxie
Configuration Manager main menu and select Devices. The Add device
from disk button can be used for installing the individual Varian ELS
Detector driver. Use this button only when directed by a Varian technical
support representative.

2.11.2 Configuring the Varian ELS Detector in Galaxie


The Varian ELS Detector driver software configuration is performed in
Galaxie Configuration Manager. Please refer to the Galaxie Configuration
Manager Operation manual for further information on how to use Galaxie
Configuration Manager.
To communicate with the Varian ELS Detector an RS232 Interface or a
RS232 PC communication bus must be configured on the acquisition
server, through Communication Engine Configuration window.
1. Select New Hardware configuration.
2. Choose RS232-PC in Hardware Type menu.
3. Configure the communication bus with the following parameters:

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Varian ELS Detector

Baud 19200 Parity None


Bits 8 Bits Flow Control None
Buffer Tx 4096 Buffer Rx 4096

Stops 1 Stop

Table 4. Bus communication parameters

4. Next, Select Systems in the Organization menu and choose the


LC system that the ELSD will be configured with. For Help on
Configuring New systems, please refer to the Galaxie
Configuration Manager Operation manual.
5. In the configuration screen at the end of the configuration
process click the button corresponding to the Varian ELSD.
6. In the Name field, select the name of the communication bus
previously configured in step 3.
7. In the Device Identifier field, enter the device identifier of the
Varian ELS detector. For example, if just one ELS detector is
connected to the system select 01. The device identifier must be
unique for each detector connected to the system (The device ID
can be set between 1-254).
8. Return to the main screen to implement the changes to the
system.

2.12 Installing the ELSD driver for ChemStation•


The Varian ELSD driver for Chemstation is only compatible with
ChemStation Rev B 03.01 or above.
To install the Varian ELSD ChemStation driver, ChemStation software (B
03.01 or later) must already be installed on the computer and you must
have administrator rights for the PC.
When you insert the Varian ELSD ChemStation Driver CD the CD browser
will start automatically. If it does not, you can launch the browser by
running Install.exe from the root directory of the CD.
From the CD browser, select “Install ELS ChemStation driver” and follow
the command prompts.
For information on how to use and configure the Varian ELSD in
ChemStation, please refer to User Guide.
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Varian ELS Detector

3. System Description and


General Operation

3.1 Basic Principles of Operation

Nebulisation
The eluent inlet is connected to the nebuliser via a short length of stainless
steel capillary tube. The incoming eluent stream passes through the heated
nebuliser and is mixed with the incoming nebuliser gas stream. The mixed
gas and eluent stream form an aerosol plume containing a uniform
dispersion of droplets that then passes as a continuous flow into the
evaporator section. Any larger droplets or the inefficiently nebulised
droplets collect in the nebuliser chamber waste trap and then drain off via
the waste outlet into a collection bottle.
Evaporation
After nebulisation the atomized spray is propelled through the evaporation
tube assisted by the carrier gas. In the evaporator section the solvent is
removed leaving a stream of dry particles of the analyte. A diffuser located
in the evaporator assists in the drying of the particles, acting as an
efficient heat exchanger, prevents ballistic particles reaching the
scattering chamber and randomizes the particle plume. The Varian ELS
Detectors use patented gas flow technology in the evaporation zone to aid
evaporation at low temperatures. By adding a stream of dry nitrogen
(evaporation gas) at the entrance of the evaporator tube less volatile
solvents (e.g. water) are easily evaporated. This evaporation gas is
controlled by the user and facilitates sub-ambient operation (Varian 385-
LC).

Detection
Light from an LED is passed through the instrument at right angles to the
direction of particle flow. A light trap is located opposite the source of
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Varian ELS Detector

light to capture the transmitted incident beam eliminating internal


reflections within the instrument body. When pure solvent is being
evaporated, only its vapor passes through the light path and the amount of
light scattered to the photomultiplier is small and gives a constant baseline
response. When a non-volatile solute is present a particle cloud passes
through the light path, causing light to be scattered. This scattered light
enters the optical aperture of the detection system and generates a signal
response from the photodiode in real time. The quantity of light detected is
dependent on the solute concentration and solute particle size distribution.

1.Nebulisation 2. Evaporation 3.Detection

Figure 3. Principles of Operation

3.1.1 Theory
.
There are four main processes by which the path of electromagnetic
radiation or light can change direction, when passing through a medium
containing a suspended particulate phase. These are shown in Figure 4:

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Varian ELS Detector

Figure 4: ELSD Scattering Mechanisms

The importance of each of these processes depends on the radius of the


particle (r) compared to the wavelength () of the incident light. Rayleigh
scattering is predominant when r/  is < 5x10-2. When particle dimensions
are greater than  /20 they no longer behave as point sources, and Mie
scattering becomes predominant. Once particle size approaches the
wavelength of incident light then reflection and refraction begin to prevail.
The relative importance of refraction and reflection can be understood by
examining the effects of the incident light on a single spherical particle
whose equilateral axis lies in the same plane as the photodetector and
light source. With this configuration, refraction is of greater significance
than reflection. The majority of organic compounds have refractive indices
between 1.3 and 1.5. Changes in the refractive index within this range will
not greatly affect the quantity of light reaching the detector. This accounts
for similarities in the sensitivity of the instrument to various compounds.

3.2 Operational Parameters


The Varian ELS Detector responds to all compounds that are less volatile
than the mobile phase and is independent of a compound’s optical
properties. It therefore provides advantages over other spectroscopic
detectors for detecting compounds that are deficient in a UV chromophore
or fluorophore.

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Varian ELS Detector

The removal of aqueous mobile phase within an ELSD is typically achieved


by setting the evaporator temperature to the eluent’s boiling point (e.g.
100 ƒC) in order to remove the solvent. For non-volatile compounds,
operating at these high temperatures maximizes the signal response.
However, at these temperatures volatile and semi-volatile compounds are
destroyed and are not detected. This is problematic for small molecules,
such as pharmaceuticals and drug candidates.
The Varian ELS detectors are specifically designed to evaporate difficult
solvents at ambient and sub-temperatures in order to maximize detection
of semi-volatile compounds.
The Varian ELSD has patented technology that reduces the evaporation
time of highly aqueous solvents at low temperature, and also prevents the
evaporation tube becoming saturated, which would otherwise preventing
further evaporation occurring.
Using this patented evaporation gas technology, a 20 †m droplet of water
at 30 ƒC can be dried ca.3x faster than just temperature alone. Using the
Varian 385-LC, water can be evaporated as low as 20 ƒC, providing
maximum sensitivity to thermally sensitive compounds. For maximum
sensitivity of non-volatile compounds the evaporation gas can be turned
off at higher evaporation temperatures.
Therefore, unlike other ELS detectors, where the evaporator temperature is
set according to the type of mobile phase, the Varian ELS detector
evaporator temperature is independent of the mobile phase. Consequently,
the Varian ELS detector can be set at 30 ƒC for all types of mobile phase
provided the evaporator gas flow is adjusted accordingly. This method of
operation ensures that the ELSD sensitivity is maximized even for low
molecular weight compounds.

3.3 Instrument Controls


The Varian ELS Detector can be used as a standalone detector via the front
keypad and screen, as shown in Figure 5.

3.3.1 Display Screen


The graphical interface on the front of the instrument displays the current Mo Mo
method, status, evaporator temperature, nebuliser temperature, gas flow
and output of the instrument. Operating parameters can be altered via the
interactive menu bar at the bottom of the display.

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Varian ELS Detector

Figure 5: Varian ELSD Display Screen

3.3.2 Keypad
The four arrows on the front of the instrument are used to navigate within
the interactive menu bar. The AZ/Stop key has a dual function; it can be
used to auto zero the ELSD at any time, unless a timetable is running. If
the AZ/Stop key is pressed during an active timetable, the timetable will
stop running and the ELSD will revert to STANDBY mode.

3.3.3 Main menu bar

To change the current settings, use the arrow keys to navigate across the
interactive menu bar until the desired option is flashing. Using the
up/down arrow keys alter the parameter to the desired setting. In order to
action any changes, the cursor must be returned to the “Home” position
( or ).

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Varian ELS Detector

When the cursor is located in the “Home” position, the actual detector
values are displayed in the main screen. If the instrument is controlled via
PC software, then the home key will display a locked icon  and the
keypad will be disabled. To unlock the keypad, software control must be
terminated.

3.3.4 Sub- Menu Screen

The sub-menu screen, which is accessed from the front screen by selecting
the  symbol and then pressing the  arrow key, allows changes to the
following electronic parameters:
PMT ---------------------------- Signal Gain
SMTH ------------------------- Time Constant
LED ---------------------------- Light Source Intensity
PWR MODE ----------------- Status at Power up
HZ ------------------------------ Data Output Rate
For more detail on each of these features please refer to Section 3.4.5
through to Section 3.4.9.

3.3.5 Status Mode

The Varian ELS Detector can be operated in two modes; STANDBY or RUN,
both of which are described below:
To display the current mode and/or select a new mode, highlight the MODE
function on the instrument display. The current mode will now be
displayed on the screen. Using the  keys, scroll up or down until the
desired option is displayed. The instrument acknowledges the command by
displaying the mode of operation in the top right hand corner of the
screen.

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Varian ELS Detector

3.3.5.1 STANDBY
The STANDBY mode is the “ground state” of the ELS detector, which is by
default initiated automatically after power on (default can be changed
using Power up option, pg 45). In STANDBY mode the heaters are switched
off, and the gas manifold valve is closed at power on. The STANDBY mode
gives the user a control platform in which to set-up the operational
parameters (gas flow, nebuliser and evaporator temperatures) before
switching the unit into RUN mode. The instrument will default to
STANDBY mode should an error occur on the instrument.
When the instrument is switched from RUN mode to STANDBY mode,
following a command or error, then the gas management system is invoked
and the gas flow set to a minimum flow of 1.2 SLM for 15 mins before the
gas manifold valve is closed. This minimum “blanket” gas is enough to
nebuliser and evacuate solvent should the instrument default to STANDBY
mode with solvent still flowing.

If the Instrument is left in Standby mode for longer than 15 minutes, gas
flow to the unit is stopped to minimize gas usage.
!
ATTENTION It is strongly recommend that the pump stop from the I/O connector of the
ELSD is connected to the HPLC pump to prevent solvent flooding the detector
should an error occur.

3.3.5.2 RUN
The RUN mode is the detector’s operational mode. In this mode the
instrument is controlled at the set temperatures and gas flow, and the
system is fully operational. During heating or cooling the instrument will
display NOT READY to show the system has not reached the set conditions.
When the instrument has equilibrated READY will be displayed and the
instrument is ready for use.

3.3.6 Error conditions


The Varian ELS Detector is equipped with a number of sensors and error
checking facilities to ensure safe operation. If an error is detected the
instrument gives an audible warning and a visible description of the error
condition. In event of any error condition, the unit defaults into the
STANDBY mode in which the heaters, LED & gas are turned off. A complete
list of instrument errors and remedial actions are given in the
troubleshooting section of this manual.

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Varian ELS Detector

3.3.7 Clearing an Error


Once the source of the problem has been corrected, the error message will
be cleared automatically on the instrument display and remain in
STANDBY mode. Select RUN mode to put the ELSD back into its
operational state. If the problem has not been rectified the ELSD will
repeatedly error when RUN mode is selected.

3.4 Operational Parameters

3.4.1 Method
The Varian ELS Detector has the capacity to store 10 custom definable
methods in memory. These methods comprise, evaporator & nebuliser
temperature and gas flow, which can be optimized for specific applications.
These 10 on-board methods are selected using the front keypad and
screen, via the METHOD option. The Method Editor Software utility (pg 48)
is required to edit and download the custom methods.
In addition to the 10 on-board methods, the Varian ELS Detector has a
method XXX that allows modification of the ELSD parameters to be made
without the need for software control. Method XXX allows the detector to
be used in standalone mode via the front screen and keypad.

3.4.1.1 Loading a Method


To load one of the 10 on-board methods, highlight METHOD. Using the
 keys scroll up or down to the required method number. The
instrument will acknowledge the change by displaying the method number
in the top left hand corner. Editing of this method is prohibited via the
front keypad; this can only be carried out using the Method Editor
Software (see Section 3.5.4 pg 48). The instrument is pre-loaded with 10
methods at the factory, as detailed in Table 5.

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Varian ELS Detector

Method Evaporator Temp (•C) Nebuliser Temp (•C) Gas Flow (SLM)
Number
Varian Varian Varian Varian Varian Varian
380-LC 385-LC 380-LC 385-LC 380-LC 385-LC
1 0 30 0 30 1.6 1.6
2 30 25 30 30 1.6 1.6
3 50 20 30 30 1.6 1.8
4 50 15 50 30 1.6 2.2
5 70 20 50 80 1.6 1.2
6 90 40 50 40 1.6 1.4
7 90 50 50 50 1.2 1.0
8 120 80 50 60 1.2 1.0
9 120 80 90 80 0.9 0.9
10 120 80 90 90 2.8 3.0

Table 5. Ten Control Methods pre-loaded on the Varian ELS Detector

3.4.2 Evaporator Temperature


The evaporator temperature is the most important setting on the ELS
detector. This should be set according to the volatility of the compound(s)
being analyzed.
If the compound is non-volatile, e.g. sugars, then the evaporator
temperature should be set to 80-90 ƒC.
If the compound is semi-volatile, or has a low molecular weight, e.g.
pharmaceutical drug, then the evaporator temperature should be set
between 20-30 ƒC.
The evaporator temperature ranges for the Varian ELS models are as
follows:
Varian 380-LC …………………….OFF, 25-90 „C (1 „C increments)
Varian 385-LC………………….….OFF, 10-80 „C (1 „C increments)

The default evaporator temperature for both models is 30 „C.

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Varian ELS Detector

3.4.3 Nebuliser Temperature


The nebuliser temperature can be used to optimize signal response in
addition to evaporator temperature. Higher nebuliser temperatures
increase peak response, but the nebuliser temperature must not exceed the
boiling point of the mobile phase.
The nebuliser temperature range for both models is: OFF, 25-90 ƒC (1 ƒC
increments).
The default value is 30 ƒC.

3.4.4 Evaporator Gas Flow


The evaporator gas flow is used to control the ELS detector’s evaporation
process. The evaporator gas value is set according to the mobile phase
composition, with higher gas flows (e.g. 1.6 SLM) being used for aqueous
eluent compared to those containing organic solvents.
The higher the evaporator temperature the lower the evaporation gas
setting required (e.g. 1.0-0.9 SLM), regardless of mobile phase composition.
Likewise, as the evaporator temperature is reduced to ambient and sub-
ambient temperatures, the gas flow needs to be increased to compensate
(e.g. 1.6-1.8 SLM).
The evaporation gas range for both models is: 0.9-3.25 SLM (0.05
increments).
The default value is 1.6 SLM.

3.4.5 Detector Gain (PMT)


This parameter sets the factor by which the detector output signal is
amplified. The gain setting does not change the sensitivity of the detector,
but merely amplifies or divides the captured signal by the inputted factor.
The gain can be adjusted from 1 to 10 in increments of 0.1.
When setting the PMT (or Gain), both the signal and noise are simply
amplified by the value set, so S/N values are unaffected. The raw signal
output displayed on the parameter screen will reflect this increase or
decrease in signal amplification.
Please note that the instrument output displayed on the main operating
screen does not alter following a PMT change, thus the recorded baseline
position will remain unchanged. Confirmation of a PMT change will be
obvious by the change in baseline noise.

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Varian ELS Detector

3.4.6 Response Time (Smoothing)


The data outputted from the detector can be averaged to produce a
smoother response. The smoothing width is set to the number of data
points over which the data is averaged and can be regarded as a digital
time constant. The smoothing range is settable from 1-50, (in increments
of 1) which translates to 0.1-5.0 secs.
For most HPLC applications the default value of 30 (3 secs) is satisfactory.
However for faster separations where peak widths <3 secs, a setting of
1(0.1 secs) is recommended.
For GPC applications where peak widths can be >30 secs, a value of 50 (5
secs) is recommended.

3.4.7 Light Source Intensity (LED)


The detector’s LED intensity can be adjusted in order to bring the peak
response back on-scale. The intensity range can be set between 0-100%,
with the default factory setting being 100%, for maximum sensitivity. The
LED setting is stored in memory and is retained even after a power on/off
cycle.
This feature is extremely useful for preparative chromatography where
samples of high concentration can be analysed which would otherwise
exceed the dynamic range of the detector.
Please note that the instrument performs an automatic auto-zero (i.e.
10mV) following an LED change in order to keep the signal on-scale.

3.4.8 Power Mode


The instrument can be configured from the front panel sub-menu (see
Section 3.34, pg 40), to start in either RUN or STANDBY mode when the
unit is switched on via the rear power button.
To configure the Power Mode, select the required Status Mode (i.e.
STANDBY or RUN) you wish the unit to start-up in from the sub menu
screen (see Section 3.3.4, pg 40). Switch off the instrument and wait for at
least 10 seconds before switching the unit back on, in order for the change
to take affect. If RUN mode is selected as the desired Power mode, then
the instrument will use the operating parameters stored in memory. In the
unlikely event that the instrument encounters a fault during power-up the
unit will automatically switch to STANDBY mode.

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Varian ELS Detector

3.4.9 Data Output Rate (Hz)


The rate at which the Varian ELS Detector outputs data can be selected
from the sub-menu screen. A 10Hz output rate is selectable for standard
LC applications, whilst a 40Hz output rate can be chosen for faster LC
separations. The data rate is stored in memory and is retained even after a
power on/off cycle. The default value is 10Hz.

3.5 Controlling the Varian ELSD Using the Standalone Software


Utilities
These Windows™-based graphical interfaces offer a second and
complementary level to total detector control. An intuitive single control
panel provides simplistic control as well as a comprehensive monitoring
system. Operational parameters can be easily manipulated, saved or loaded
by using the flexible Methods Editor enabling rapid set-up and custom
method archiving.

A general description of the features available through the software


utilities is given below, but for a more comprehensive guide on how to use
the control software, please refer to the on-line help supplied with the
software.

3.5.1 Control Software-Overview


Control of the Varian ELSD is achieved through the simple control window.
Within the control window, the status of the detector is displayed,
together with options to control the various instrument parameters. The
control window is effectively divided into three main sections:

1. Control Window
View the current mode of operation
Change the current mode of operation between
STANDBY and RUN
Change the current Method of operation between a
stored custom method and the default method ‘XXX’
Change detector parameters directly via method ‘XXX’

2. Status window
Displays the actual values against the set point for:
i. Evaporator Temperature
ii. Nebuliser Temperature
iii. Gas Flow

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Varian ELS Detector

3. Photodetector window
Displays current detector output
Displays current gain setting
Auto-zero the detector

Figure 6: Control Software Main Screen

3.5.2 Control Software-Parameter Settings


All of the six basic instrument control parameters can be modified via the
instrument control panel. Changes to temperature and gas flow are made
via the METHOD button, whilst changes to the LED, Smoothing and Gain
are adjusted via the Edit menu: - (EDIT / Instrument settings menu option).

Once a change has been made, the UPDATE button must be pressed in
order to download the information to the detector.

Note: The L.E.D intensity is set for ALL methods used on the detector and is NOT
Method specific.

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Varian ELS Detector

3.5.3 Control Software-System Test


The System Test is used to evaluate the Varian ELS detector’s performance,
to ensure it is operating to the high standards set by Varian. When you
select this feature (TOOLS / Run system test menu option), the software
will run the ELSD through a number of internal diagnostic tests, and then
compare the results with the expected values set by Varian. The test
information can subsequently be printed as a record.

Please note that the test takes approximately 2 hours to complete and
should only be used occasionally to check the instrument’s performance, or
when a problem is encountered.

3.5.4 Method Editor Software-Overview


The Varian ELSD can store 10 custom methods, which can be selected via
the front of the instrument or via the control software. A custom method
consists of nebuliser, evaporator and gas flow settings.
The method editor program allows the user to create, edit and download
these custom methods for method development purposes or specific
applications. The method editor program can be launched from the control
software via the “Launch Method Editor” icon.

Figure 7: Control Software Main Screen


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Varian ELS Detector

3.5.5 Method Editor-Creating & Storing Methods


To change a custom method on the Varian ELSD, you must first create a
custom "Method Set", (FILE/New). A Method Set comprises 10 custom
methods, which can be customised using the Metho Editor software. A
description can be entered for each method within the method set in order
to distinguish between them.
Having created a method set, the set of methods can be downloaded to the
ELSD via the DOWNLOAD button.
Single methods within a method set cannot be individually downloaded to
the detector. All 10 methods of the Method Set must be downloaded
simultaneously to the Detector.
Each Method Set can be saved as an individual binary format file with a
File Extension (.ELS). By default, saved Method Set files are stored in the
Method folder allocated at the time the software was installed (C:\Varian-
ELSD\default).
Alternatively, a loaded Method Set can be printed by selecting the print
option from the FILE menu.

3.5.6 Method Editor-Downloading Method Sets


To download a Method Set to the Varian ELSD, open the desired Method
Set to be downloaded.
Ensure the Method Editor is configured for the correct
communication port for the detector.
Ensure that any software session that is currently accessing the
detector via the selected COM port is closed down.
Select the DOWNLOAD button to send the methods to the ELSD.
If the download was successful, you will see a dialog saying: "ELS Updated
OK".
If the download was unsuccessful, you will see the following dialog:

In this case, check that the detector is connected to the PC, is switched on,
and the service switch is in the up position (RUN).
A comprehensive guide on how to use the Method Editor program can be
found in the on-line help supplied with the software
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Varian ELS Detector

3.6 Controlling the Varian ELSD During an Injection


The Varian ELS Detector has the capability to change operational
parameters in real-time, during a sample injection, using an on-board
timetable.

3.6.1 Real-time operation


The Varian ELS Detector can store in memory a series of time-based events,
within a single timetable. This timetable allows the operational settings of
the ELSD to be changed in real-time during a run.
The temperatures, gas flow, LED, gain and smoothing parameters can all be
configured within this timetable to change during a sample injection.
The timetable can be used to program the gas flow, in order to compensate
for the change in ELSD response across a solvent gradient. Alternatively,
the timetable can be customized to create adjustable LED intensities across
a sample injection for mixtures containing samples with wide
concentration ranges.
The single timetable, stored on-board the ELSD, is only customizable using
the Varian ELSD DIMENSION software, which can be purchased from Varian
(Part No. PL0890-0375).

3.6.2 Creating a real-time program


In order to create or modify the on-board timetable, DIMENSION software
must be installed on your PC.
The DIMENSION software package allows you to create a timetable on a
PC, which can subsequently be downloaded to the ELSD for later use.
The ELSD can only store a single timetable in memory, so the DIMENSION
software can be used to create & save multiple timetables that can be
downloaded individually at a later date.
For further information on how to use DIMENSION software, please refer
to the DIMENSION software on-line help.

3.6.3 Starting & stopping real-time control


` The ELSD contains an internal timer to initiate the time-based events
stored within the timetable. To start the internal timer and trigger the on-
board timetable a contact closure input via the I/O connector on the rear of
the instrument is required (see Section 2.5, pg 24).

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Varian ELS Detector

When the on-board timetable is triggered, the front panel of the ELSD will
display “TTRUN” above the output, as shown in Figure 8

1 2
3

1. Current runtime
2. Total runtime
3. On-board Timetable is active
Figure 8: Varian ELSD front panel display during timetable operation
When the timetable is running, the current and the total run time are
displayed, in minutes, at the top-centre of the ELSD display.
When the timetable reaches the end of its run time, the ELSD will revert to
RUN mode and be primed ready to start the timetable again.
During an active timetable, where the evaporator temperature is being
controlled, the status of the instrument will change from READY to NOT
READY. This is normal behavior and will not affect the running of the
timetable.
The STOP button on the instrument’s front keypad can be used to interrupt
the active timetable whilst it is running. When the STOP button is pressed
the instrument will revert to STANDBY mode.

3.7 Controlling the Varian ELSD Using Galaxie


In order to control the Varian ELS Detector using Galaxie Chromatography
Software, the appropriate ELSD driver must be installed. Please refer to
Section 2.9, (pg 30) for instructions on how to install the Galaxie ELSD
driver software.

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Varian ELS Detector

3.7.1 Galaxie Status window


Within Galaxie’s main menu screen, direct control of the instrument can be
accessed via the instrument icon.

In this status window, the detector’s output and control parameters


(nebuliser, evaporator, gas flow, etc.) are shown with their current values,
depending on the control method program.
When the RUN button is selected, the detector will begin heating to the
set temperatures and gas flow. When the detector is heating the light will
turn orange. When the detector has reached the set parameters, the light
will turn green.
When STANDBY button is selected, the detector’s LED will turn off, along
with the heaters. The gas flow will revert to a minimum value of 1.2 SLM.
When this function is active, the indicator light turns solid red.
The detector can be auto zeroed from this screen at any time, by pressing
the AUTOZERO button.
To set the detector parameters, click on the CONFIGURE button to access
the parameter configuration screen, as shown:

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Varian ELS Detector

In the configuration men, the following detector parameters can be set and
downloaded to the detector.
Parameter Operational Range
Evaporator Temperature
Varian 380-LC Ambient –120 ƒC
Varian 385-LC 10-80 ƒC
Nebuliser Temperature Ambient – 90 ƒC
Gas Flow (SLM) 0.9-3.25
Gain 1-10
Smoothing 1-50 (i.e. 0.1 to 5 secs)
LED (%) 0-100
Note: Galaxie will automatically adjust the evaporator range according to
the model of ELSD connected.
Once the detector parameters are set, press the OK button to download the
values to the detector. The detector parameters cannot be adjusted during
data acquisition.

3.7.2 Galaxie Connection status


When the Varian ELS Detector is connected to Galaxie Chromatography
Software, the detector’s firmware version (e.g., 22.0.4) is shown at the top
left corner of the configuration screen. If communication is lost, or no ELS
detector is connected, “offline” is shown.

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Varian ELS Detector

3.7.3 Galaxie Status Overview


A general overview of the HPLC system and current status of the ELS
detector can be accessed via the OVERVIEW button, within Galaxie’s main
menu screen.
The overview screen displays a graphical representation of the ELSD; along
with the read-back values of the detector’s key parameters.

The status of the detector is indicated in the top left hand corner, with the
green RUN light.
When the Varian ELSD encounters an error it will switch to STANDBY
mode, the status light will turn red and an error code message will be
displayed on-screen. The error is also recorded in the Galaxie Events menu.
A complete list of instrument errors and remedial actions are given in the
troubleshooting section of this manual. Select RUN mode to clear the error
and continue operating the detector. If the detector error is still present,
the ELSD will show an error message as soon as the unit is put back into
RUN mode.
The current detector temperatures and output are also displayed in the
screen, for easy reference and the detector can also be Auto zeroed from
this overview screen.

3.7.4 Automating the Varian ELS Detector


Galaxie Software can be used to automate the operation of the Varian ELS
Detector, using methods and sequences. To create a Galaxie method or
sequence, please refer to the Galaxie User’s Guide.
In the control section of the system method press the instrument icon
button to display the ELSD control parameters.

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Varian ELS Detector

The method parameter window allows the ELS detector conditions to be


changed according to a time-based program. For example, the gas flow
parameter can be altered across a sample injection in order to control
detector response.
To create a time-based program, enter the time, when you want a change
to take place, and the desired detector conditions across each line.
Additional lines can be added, deleted or the whole table erased by using
the table formatting buttons on the right.
The detector can also be autozeroed automatically between instrument
methods if the “Autozero on Method Change” is selected. Alternatively, the
instrument can be shutdown after an injection, or sequence if the “Go to
Standby at End of Run” option is selected.
For greater control and flexibility in changing ELSD parameters during an
injection see section 3.6 (pg 50).

3.8 Controlling the Varian ELSD within ChemStation•


The Varian ELS Detector can be controlled directly via ChemStation, Rev
B.03.01, along with digital data acquisition, without the need for an A/D
interface. Controlling the Varian ELSD within ChemStation provides full
detector functionality with the added benefit of remote automation.
The Varian ELSD Driver for ChemStation can be purchased from Varian (Part
No. PL0890-0380).
In order to control the Varian ELSD via ChemStation Rev B.03.01, the
Varian ELSD control driver must be installed onto the PC running
ChemStation. Please refer to the Varian ELSD Control for ChemStation
manual on how to install the ELSD ChemStation driver.
Note: The ChemStation driver does not provide control for the PL-ELS 1000.

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Varian ELS Detector

3.9 General Considerations


The Varian ELS Detector should be thought of as a detector like any other
designed for liquid chromatography. The main distinguishing feature is the
ability to evaporate the solvent from the column eluent. Therefore, normal
system set-up precautions should be remembered when starting to use the
instrument. Any solvent intended for use with the Varian ELSD should be
fully miscible with any previously used in the liquid chromatograph; if
there is any uncertainty, then a mutually miscible solvent should be run
through the system as an intermediate liquid. The sample loop should also
be flushed with miscible solvent where necessary. The intended eluent
should be thoroughly degassed, contain no non-volatile salts or material
and should be fully compatible with the column(s). All connections should
be made with zero dead volume fittings and tubing with an I.D.  0.010”.
The Varian ELSD requires nitrogen of purity >98%, at an inlet pressure of
60-100 psi. If in-house nitrogen is not available then we recommend the
use of a nitrogen generator a constant uninterrupted supply of high purity
gas. Air can be used with non-flammable solvent systems. The eluent of
choice should be fully volatile under the chosen detector parameters – any
non-volatilized eluent will increase baseline noise and reduce sensitivity.
The ELS Detector is a destructive technique and must be placed last when
used in series with other detectors.

3.9.1 Solvent recommendations


Any solvent intended for use with the Varian ELS Detector should be
thoroughly degassed, filtered (0.45 †M) and fully compatible with the
column(s). Solvents that are not properly degassed may cause problems at
nebulisation leading to a poor reproducibility.
Non-Volatile buffers are not compatible with the Varian ELS Detector and
should not be used. Only volatile mobile phase additives, such as those
listed in Table 6 (pg 57) should be used with the ELS detector.
Tetrahydrofuran (THF) stabilized with BHT, may increase the baseline noise
level. Where possible unstabilised THF should be used with the ELS
detector.
High boiling point solvents such as N-methylpyrrolidinone (NMP),
Dimethylsulphoxide(DMSO), Dimethylacetamide (DMac), m-Cresol and
1,2,4, Trichlorobenzne (TCB) are not recommended for long-term operation.
Greater care and attention to instrument cleaning procedures should be
exercised with these solvents.
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Varian ELS Detector

3.9.2 Sample preparation


Samples containing particulate matter should be filtered through a 0.45
†m filter prior to injection.
Mobile Phase Additive pKa pKb pH Range Bp (•C) Mp (•C)
Acids
Trifluoroacetic Acid (TFA) 0.3 13.70 72.4 -15.4
Formic Acid 3.75 10.25 100.7 8.3
Acetic Acid 4.75 9.25 116.0 16.6
Bases
Ammonia 9.25 4.75 -33.4 -77.7
Methylamine 10.66 3.34 -6.6 -94.0
Ethylamine 10.81 3.19 16.6 -81.0
Triethylamine 11.01 2.99 89.3 -114.7
Buffers
Ammonium Formate 3.8, 9.2 3.0-5.0 120
8.2-10.2
Ammonium Acetate 4.8, 9.2 3.8-5.8 111
8.2-10.2
Ammonium Bicarbonate 6.3, 6.8-11.3 106
9.2,
10.3
Ion-Pair Reagent
Pentafluoropropionic acid (PFPA) ~0.6 97
Heptafluorobutyric acid (HFBA) ~0.6 120
Nonafluoropropionic acid (NFPA) ~0.6 140
Tridecafluoroheptanoic acid ~0.6 175

Table 6. Volatile mobile additives compatible with ELS detection

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3.9.3 Column Considerations


The ELS detector will detect all non-volatile components in the mobile
phase, which includes column-packing material. Column packing material
will become chemically and mechanically broken down over the lifetime of
the column, causing particles to enter the ELSD. This column “shedding”
will lead to extremely high baseline noise levels.
Amino columns used with aqueous mobile phase are particularly prone to
this type of shedding and should be checked regularly. To minimize column
breakdown always follow the manufacturers instruction supplied with the
column.

3.9.4 Transferring ELSD Methods


The direct transfer of ELSD operating conditions from other manufacturers’
ELS detectors, or other designs of ELSD (e.g. PL-ELS 1000) to the Varian
ELSD will not provide equivalent performance.
As stated in Section 3.1(pg 35), the operating temperatures of the PL-ELS
Detector are set according to the type of analyte and not the mobile phase
composition as with other ELS detectors. For example, the PL-ELS 1000 has
to operate at temperatures above 90 „C for a mobile phase of water;
whereas the Varian ELSD can operate at 30 „C for the same mobile phase.
Therefore the transfer of operating conditions from other models of ELSD
to the Varian ELSD is not valid and the only way to ensure that the
detector will provide the optimum analyte signal-to-noise is to follow the
guidelines outlined in Section 3.4, pg 42.

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4. Routine Maintenance

Trained personnel only should carry out maintenance inside the unit. There
are no user-serviceable parts inside the instrument. Unauthorized access to
the instrument will invalidate the instrument warranty.

Warning
When disconnecting tubing from the instrument, solvent may leak out.
Please observe appropriate safety procedures (e.g., safety glasses,
gloves and protective clothing) according to the safety data sheets
when handling solvents.

The Varian ELS Detector is designed to be a low-maintenance instrument


and does not generally require regular service. However, should the
instrument performance deteriorate, we recommend the following
procedures to clean the nebuliser and evaporator section without
dismantling the unit.
If cleaning the unit does not fix the problems then consult Varian for
further assistance.

4.1 Drying the Diffuser


If the instrument has been operated incorrectly the diffuser may become
blocked with liquid. This is manifested by loss of signal, increased baseline
noise and in the extreme case gas bubbling out of the nebuliser drain tube.
If this happens then simply turn off the liquid flow, increase the gas flow
to 2.8 SLM and increase the evaporator to maximum temperature. The
diffuser will be dried out and the instrument ready to use after
approximately 1 hour under these conditions. Reset the instrument to the
correct operating conditions and allow to stabilize before continuing.

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4.2 Cleaning Evaporator Tube


If the evaporator tube becomes contaminated with non-volatile material
resulting in poor chromatography, it is recommended that the instrument
is initially washed with a solvent suitable for the contamination. To
perform this wash, pump the appropriate solvent into the instrument at 1
to 2 mL/min whilst the instrument is in RUN mode. Following this
procedure, dry out the instrument by running the system at maximum
temperatures, without eluent flow. To clean a unit, set the evaporator
temperature to 80 ƒC, the nebuliser temperatures at 60 ƒC and the gas
flow to 2.8 SLM. Pump a mixture de-ionized Water/Acetone (50/50) at 1
mL/min (whilst in the RUN mode) overnight, or for a minimum of 4 hours if
overnight operation is not possible. Depending on usage, it is
recommended to clean the evaporator tube once a week or every 40 hours
of use as a preventative routine. It is also recommended to clean the unit
following the use of buffers.

Do not use eluents that contain additives when performing the cleaning
!
ATTENTION
procedure.

ENSURE THAT THE INSTRUMENT IS AT EQUILIBRIUM UNDER THE ABOVE


! CONDITIONS BEFORE LEAVING THE INSTRUMENT UNATTENDED.
WARNING
If cleaning the unit does not cure the problems then consult Varian, Inc.
for further assistance.

4.3 Information for Service Personnel

! INSTRUMENT IS DOUBLED FUSED.


WARNING

4.3.1 Heater PCB Fuses


There are 3 fuses fitted to the main control PCB, one to protect each of the
heater circuits.
FH 1 & 3: H 1A FF 250V
FH 2: TR5 2A T 250V

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4.3.2 Light Source


The light source assembly is a Class 1 LED product as defined in IEC 60825-
1 Ed 1.2. Whilst this is non-hazardous it is advisable to avoid staring into
the beam.

4.4 Putting the Instrument into Storage


If the instrument is to be stored or not used for a period of time it is
recommended to follow the procedure outlined below:-
1. Flush the detector with a mixture of Acetone/Water (50/50) at 1
mL/min for 15 mins.
2. Allow the instrument to cool to ambient temperature in STANDBY
mode with the gas supply still connected.
3. Tip the instrument forwards to try and empty the 'P' trap contents
through the front waste tube (i.e. into the bottle).
4. Pour 10 to 20 mL of acetone into the exhaust tube to flush out the
solvent trap, collecting the waste in the waste bottle at the front
of the instrument.
5. Again tip the instrument forwards to drain the solvent trap.
6. Disconnect the waste bottle.
7. Using the gas supply, blow nitrogen gas through the exhaust to
evaporate any remaining acetone in the solvent trap. Cover the
waste tube with tissue paper to collect any acetone residue.
8. Plug the exhaust, waste tubes and solvent inlet with the plastic
caps provided.

4.5 Upgrading the Firmware

4.5.1 Tools required


The tools required to replace the flow cell are:
 A copy of HEXTERM.exe or Terminal.exe (both available from Varian).
 A copy of the latest Varian ELS Detector firmware appropriate to
model.
 Serial cable supplied with instrument (Part No. PL 0890-0325).

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4.5.2 Firmware upgrade procedure


To upgrade the firmware:
1. Close down any software currently connected to the unit and turn
off the instrument.
2. At the rear of the detector move the switch, located below the
serial connector, to the up position.
3. Run the HexTerm.exe program.
4. Select the Varian ELS Detector from the menu bar and the correct
communication port.
5. Turn on the instrument and check that the message, “Bootloader
v904211”, is shown.
6. Browse to select the new firmware (e.g. A:\9061_22.04.hex).
7. Select the download icon, to upgrade the EPROM with the new
firmware. During transfer, the auto-zero light on the detector
front panel will turn red and flash.
8. On successful completion of the programming, a message will
appear and all three lights on the front panel will turn green.
9. Exit the HexTerm program and turn off the instrument.
10. On the back of the Varian ELS Detector move the switch, located
below the serial connector, to the down position.
11. Switch the detector back on and check the version of firmware in
Galaxie by choosing the status option in the Varian ELS Detector
control window.

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5. Troubleshooting

If a problem is encountered Varian, Inc. advises that a system test be


performed via the ELS standalone control software (Section 3.5.3, pg48) to
ensure that the detector is working correctly. If there is an error or fault
and you follow the recommended course of action and the result is not
satisfactory, then please direct the matter to Varian, Inc. or your local
distributor.
Malfunctions within the Varian ELS Detector can arise from three general
sources:
 The Varian ELS Detector itself can be dirty or operating outside
specification.
 The HPLC system can have a broken, dirty, or non-optimally operating
component, but the problem is manifesting itself in the Varian ELS
Detector.
 A mobile phase and/or column problem, which by its very nature is
spread throughout the HPLC system but appears as a malfunction of
the Varian ELS Detector.
To troubleshoot the Varian ELS Detector, you must be able to separate the
performance of the ELS Detector within the HPLC system from its
performance outside the HPLC system. This section begins with guidelines
for testing the Varian ELS Detector as a stand-alone. The troubleshooting
Table on pg 65 lists the observed problem with the possible cause and the
suggested solution.

5.1 Troubleshooting an HPLC System


As you go through the troubleshooting table, you will have occasional
instructions for HPLC systems. Standard practice is to add one component
at a time back into the HPLC system so that the component causing the
problem is easily identified if/when the condition reoccurs.
Begin troubleshooting by adding the pump to the Varian ELS Detector first
and finish by adding the column last. If another type of detector is
available use it before the Varian ELS Detector to aid in troubleshooting.

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5.2 Instrument Errors


Error condition Description Suggestions
Environmental temp too cold. Move to
10 Air temp <= 10 ƒC inside enclosure
warmer location
Environmental temp too hot. Move to cooler
11 Air temp > 40 ƒC temp inside enclosure
location
12 On-board sensor heater failed Vapor sensor needs replacing
Check vapor sensor on rear of ELSD is not
13 Rear panel sensor heater failed
damaged/ Vapor sensor needs replacing
14 Leak detected inside unit Stop pump and investigate
Liquid leak sensor has detected liquid in
15 Stop pump and investigate
drip tray
Fault with the circuitry / wires / fan Call
16 Fan driver IC thermal shutdown
service engineer if this happens regularly
Fault with the circuitry / wires / fan Call
17 Fan stopped
service engineer if this happens regularly
Nebuliser temperature exceeded
18 Faulty thermocouple or heater control
threshold after stabilizing
Evaporator temperature exceeded
19 Faulty thermocouple or heater control
threshold after stabilizing
20 Light source error Replace light source assembly
Evaporator gas flow rate exceeded Check operating head pressure, otherwise
21
threshold after stabilizing faulty mass flow controller
Invalid nebuliser temp reading (FAULTY
22 Replace nebuliser heater assembly
RTD)
Invalid evaporator temp reading (FAULTY
23 Replace evaporator assembly
RTD)
Fault with the peltier unit. Call service
24 Fan failure on cooled evaporator
engineer if this happens regularly
Evaporator tube current outside of normal Fault with the peltier unit. Call service
25
range engineer if this happens regularly

Table 7. Instrument errors

64 Publication date: February 2008


Varian ELS Detector

5.3 General Problems


Faults or Problems Possible Cause(s) Remedy
Baseline noise 1. Poor nebulisation of solvent Increase the temperature of the
evaporator by 10ƒ intervals until the
2. Insufficient evaporation
noise is acceptable
3. Non-volatile additive in mobile
Increase the evap gas flow rate
phase
Decrease the nebulisation
4. Pressure difference created inside
temperature
nebuliser chamber
Ensure that the end of the liquid
5. Pump pulsations, especially in
waste tube is not immersed in liquid
microbore applications where low
flow rates are used Ensure that the exhaust tube at rear
of unit is not blocked, or extraction is
too strong
Use a pulse free pump
Increase the back pressure on the
pump by fitting a back pressure
column between the pump and the
injection valve
Use a pulse dampener directly after
the pump in the system
Use a volatile mobile phase as shown

Baseline spikes Particulate matter in the gas supply Filter the incoming gas, or change the
supply
Column shedding
Replace column or fit an inline filter
Poor nebulisation
with a 0.2 †m membrane filter
Non-volatile additive in mobile phase directly after the column
Replace additive in mobile phase with
volatile buffer
Low sensitivity and Diffuser saturated with solvent Stop the eluent flow and increase the
baseline noise/drift evaporator temperature to
50 ƒC above the current set
temperature. Increase the flow rate to
2.8 SLM and wait 1 hour

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Varian ELS Detector

Large Baseline offset Inefficient evaporation Increase the evaporator temperature


and/or gas flow
High concentration of non-volatile
buffer or stabiliser Use a lower concentration of
stabiliser, unstabilised solvent or a
Contaminated diffuser
more volatile buffer (ammonium
Optics Heater failed acetate or ammonium formate)
Perform cleaning procedure
Refer to local distributor or Varian,
Inc.
Peak tailing 1. Eluent particles lingering in the Increase evap gas flow rate
optical chamber
Adjust HPLC separation
2. Poor chromatography
Instrument Fails to Offset too high or output unstable Stop pump flow and switch off unit.
zero due to impurity in mobile phase Restart unit and A/Z without liquid
flowing
Refer to local distributor or Varian,
Inc.
No power Mains lead not connected Attach mains lead to socket and inlet
on rear of instrument
Fuse failure
Replace fuse
No response Data acquisition leads not connected Ensure connectors to computer or
(completely flat integrator are sound
Light source inactive
baseline)
Check LED intensity is 100%
Output below 0 mV
Stop pump flow and A/Z without
Instrument in STANDBY mode
liquid flowing
Service switch in Flash mode
Select RUN mode
Ensure Switch is in UP position
Temperature error as Temperature probe fault or Check RTD connections
soon as instrument disconnected
Consult Varian Inc or your local agent
powered on
for further advice
Display not on, but Instrument in service mode Ensure service Switch is in UP position
power connected, (RUN)
blue glow ON
Consult Varian, Inc. or your local
agent for further advice

66 Publication date: February 2008


Varian ELS Detector

Evaporator Peltier cooler has not initiated Switch detector off then on at the
Temperature reads correctly power socket
zero at start-up and
Consult Varian, Inc. or your local
cannot be changed
agent if problem persists

Vapour sensor error Solvent vapour near the front of unit Remove any solvent bottle or solvent
occurs, but there is no is being drawn into the unit leak that is directly in front of the
solvent or vapour leak detector
inside unit
Check the rear vapour sensor is not
Faulty Vapour sensor
damaged/bent
Varian 385-LC Ambient temperature too high Reduce ambient temperature to 25 ƒC
Evaporator will not
Consult Varian, Inc. or your local
reach low
agent if problem persists
temperature e.g. 10 Faulty Peltier cooler unit
ƒC

Table 8. General problems and remedies

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Varian ELS Detector

APPENDIX 1 – Method Record

Chromatography Eluent Eluent Method Evap Neb Gas Date Comments


Conditions Flow Number Temp Temp Flow
Stored

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Varian ELS Detector

APPENDIX 2 – Spare Parts Listing

The following list of spare parts was current at the time of issue of this manual. Please
contact your local distributor or Varian for an up-to-date price list and availability.
Description Part Number
Analogue Output Cable PL0890-0300
Gas Inlet Tube (2 m) PL0890-0305

Exhaust Hose (PVC-2.0 m) PL0890-0310


Waste Hose (Tygon) 7 cm PL0890-0315
Solvent Waste Container (500 mL) PL0890-0320
RS232 Communication Cable PL0890-0325
Varian ELSD Mains Lead (UK) PL0890-0330
Varian ELSD Mains Lead (EURO) PL0890-0335

Varian ELSD Mains Lead (US) PL0890-0340


I/O cable PL0890-0345
Remote Start Cable PL0890-0350
Varian ELSD Operation Manual PL0890-0355
Varian ELSD Service Manual PL0890-0360
Varian ELSD IQ/OQ Workbook PL0890-0365
Varian ELSD Control Software PL0890-0370
Varian ELSD DIMENSION Software PL0890-0375
Varian ELSD driver for ChemStation• PL0890-0380
Galaxie LC Driver Software 8510244000

Table 9. Spare parts listing To order please contact your local office.

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Varian ELS Detector

APPENDIX 3 – Cleaning and


Decontamination Procedure

Warning
Switch off and disconnect power cord from instrument before
cleaning. Allow any hot parts to cool before proceeding.

Cleaning
The exterior of the instrument should be cleaned by wiping down with a
soft cloth moistened with dilute detergent solution, followed by wiping
down with a cloth moistened with deionized water. Ensure that no
moisture enters the instrument. Allow the instrument to dry off completely
before reconnecting power.

Decontamination

Caution This procedure should only be carried out by trained service personnel
only.

The operator should wear appropriate personal protective equipment for


this operation (gloves, safety glasses, lab coat and respirator if the level of
hazard has been risk-assessed to be sufficiently high).
Disconnect the instrument completely and remove it to a fume cupboard if
necessary. Open the cover of the instrument to see if any solvent has
contaminated the interior.
Excess quantities of liquid spilt on or inside the instrument should be
mopped up using absorbent cloths, followed by repeated wiping down with
soft cloths moistened with acetone or deionized water (as appropriate to
70 Publication date: February 2008
Varian ELS Detector

the spilt solvent) until the last traces of the hazardous liquid have been
removed. If liquid has collected in the drip tray around the leak sensor, be
very careful not to damage or displace the sensor bead whilst mopping up.
Identify and if possible correct the source of the leak. Inspect cabling, parts
and surfaces to determine whether any damage has occurred. If in doubt,
contact the Varian Service Department for assistance.
Allow the interior and exterior of the instrument to dry out completely
before closing the cover and reconnecting power.
Dispose of contaminated waste appropriately.

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Page: 18
[SMB1] Not needed in packing list-can purchase as an option

Page: 18
[SMB2] Not sure on name format for this

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