ELS Detector C-650
Operation Manual
11593555 en
Table of content
1 About this manual 5
1.1 Abbreviations 5
2 Safety 6
2.1 User qualification 6
2.2 Proper use 6
2.3 Improper use 6
2.4 Safety warnings and safety signs 7
2.5 Product safety 9
2.5.1 General hazards 9
2.5.2 Warning labels on housing and assemblies 10
2.5.3 Personal protective equipment 10
2.6 General safety rules 10
2.6.1 Responsibility of the operator 10
2.6.2 Duty of maintenance and care 10
2.6.3 Spare parts to be used 10
2.6.4 Modifications 10
3 Technical data 11
3.1 Scope of delivery 11
3.1.1 Standard device 11
3.1.2 Standard accessories 11
3.1.3 Optional accessories 12
3.2 Technical data overview 12
4 Description of function 13
4.1 Overview over the device 13
4.2 Functional principle 14
4.2.1 Nebulization 14
4.2.2 Evaporation of the solvent 16
4.2.3 Detection 16
4.3 Eluent flow splitting 17
5 Putting into operation 18
5.1 Installation site 18
5.2 Electrical connections 19
5.3 Gas supply 20
5.4 Exhaust venting and drain requirements 22
5.5 Installing the nebulizer/glass chamber assembly 23
5.5.1 Connecting the siphon overflow 24
5.5.2 Connecting the nebulization gas to the nebulizer 24
5.6 Installing the flow splitter 25
5.6.1 Connecting the flow splitter 25
5.6.2 Adjusting the flow rate of the ELSD splitter 25
5.6.3 Connecting to the ELS nebulizer 26
5.7 Powering up the device 26
5.8 Control panel 26
5.8.1 Digital display 26
5.8.2 User interface 27
5.9 Initial test procedures 34
5.9.1 Preliminary activities 34
5.9.2 Electronic noise test 35
5.9.3 Background noise (stray light) test 35
5.9.4 Solvent noise test 36
5.9.5 Column noise test 37
6 Operation 38
6.1 Preparing the device for operation 38
6.2 Auto-zeroing the detector 38
6.2.1 Manual 38
6.2.2 External 39
6.3 Routine operation of the detector 39
6.4 Optimizing the performance 39
6.4.1 Selecting the optimum temperature 39
6.4.2 Optimizing the mobile phase 40
6.4.3 Sample pretreatment 41
6.4.4 Column treatment 41
6.4.5 Optimizing the noise filter 42
6.5 Powering down and shutting down the detector 42
7 Maintenance 43
7.1 Customer service 44
8 Troubleshooting 45
8.1 General troubleshooting information 45
8.2 Initial troubleshooting activities 45
8.3 Perform the noise test 46
8.4 Specific detector troubleshooting 46
8.5 Nebulizer cleaning and replacement procedures 47
8.6 Gas flow problems 49
8.7 Cleaning and decontamination 49
8.7.1 Device cleaning 49
8.7.2 Device decontamination 50
8.8 Light source exchange 50
9 Shutdown, storage, transport and disposal 51
9.1 Preparing the device for storage and transport 51
9.2 Storage and transport 51
10 Spare parts 52
11 Declarations and requirements 53
11.1 FCC requirements (for USA and Canada) 53
11.2 Declaration of conformity 54
1 About this manual
This manual describes the Low Temperature Evaporative Light Scattering Detector C-650 and
provides all information required for its safe operation and to maintain it in good working order. It
is addressed to laboratory personnel and operators in particular.
Read this manual carefully before installing and running your system and note the safety precautions in chapter 2 in particular. Store the manual in the immediate vicinity of the device, so that it
can be consulted at any time.
No technical modifications may be made to the device without the prior written agreement of
BUCHI. Unauthorized modifications may affect the system safety or result in accidents. Technical
data are subject to change without notice.
NOTE
The symbols pertaining to safety are explained in chapter 2.
This manual is copyright. Information from it may not be reproduced, distributed or used for
competitive purposes, nor made available to third parties. The manufacture of any component
with the aid of this manual without prior written agreement is also prohibited.
The English manual is the original language Version Bnd serves as basis for all translations into
other languages. If you need another language version of this manual, you can download available versions at www.buchi.com.
1.1 Abbreviations
ELSD: Evaporative Light Scattering Detector
Fig: Figure
TTL: Time to live (electrical signal)
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1 About this manual
C-650 Operation Manual, Version B
2 Safety
This chapter points out the safety concept of the device and contains general rules of behavior
and warnings from hazards concerning the use of the product.
The safety of users and personnel can only be ensured if these safety instructions and the safety
related warnings in the individual chapters are strictly observed and followed. Therefore, the
manual must always be available to all persons performing the tasks described herein.
2.1 User qualification
The device may only be used by laboratory personnel and other persons who on account of
training or professional experience have an overview of the dangers which can develop when
operating the device.
Personnel without this training or persons who are currently being trained require careful instruction. The present Operation Manual serves as the basis for this.
2.2 Proper use
The device has been designed and built for the use in laboratories. The ELSDC-650 is a standalone device. The C-650 is designed to detect compounds in the eluent from Preparative Chromatography.
2.3 Improper use
Applications not mentioned above are improper. Also applications which do not comply with the
technical data are considered improper.
DANGER
During any improper use, the effectiveness of the protection systems can be affected.
• Avoid any improper use of the devices!
The operator bears the sole risk for any damages caused by such improper use.
The following uses are expressly forbidden:
• Use of the device in rooms which require ex-protected devices.
• Use on samples which can explode or inflame (e.g.: explosives, etc.) due to shock, friction,
heat or spark formation.
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2 Safety
C-650 Operation Manual, Version B
2.4 Safety warnings and safety signs
DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying
levels of hazard seriousness of risks related to personal injury and property damage. All signal
words, which are related to personal injury are accompanied by the general safety sign.
For your safety it is important to read and fully understand the table below with the different signal words and their definitions!
Sign Signal word Definition Risk level
Indicates a hazardous situation which, if
DANGER
WARNING
CAUTION
not avoided, will result in death or serious
injury.
Indicates a hazardous situation which, if not
avoided, could result in death or serious
injury.
Indicates a hazardous situation which, if
not avoided, may result in minor or moderate injury.
★★★★
★★★☆
★★☆☆
Space for
supplementary safety
information
symbols.
★☆☆☆
(property damage
no
NOTICE
Indicates possible property damage, but no
practices related to personal injury.
only)
Supplementary safety information symbols may be placed in a rectangular panel on the left to
the signal word and the supplementary text (see example below).
Source of hazard.
Table of supplementary safety information symbols
The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Symbol Meaning
SIGNAL WORD
• List of measures to avoid the herein described, hazard or hazardous situation.
• …
• …
General warning
Electrical hazard
Heavy weight, avoid overexertion
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2 Safety
C-650 Operation Manual, Version B
Symbol Meaning
Harmful to life-forms
Pinch point. Mechanical hazard.
Fire hazard
Hot item, hot surface
Device damage
Inhalation of substances
Chemical burns by corrosives
Wear laboratory coat
Wear protective goggles
Wear protective gloves
Heavy weight, lifting requires more than one person
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2 Safety
C-650 Operation Manual, Version B
Additional user information
Paragraphs starting with NOTE transport helpful information for working with the device/software
or its supplementaries. NOTEs are not related to any kind of hazard or damage (see following
example).
NOTE
Useful tips for the easy operation of the device/software.
2.5 Product safety
The ELSD is designed and built in accordance with state-of-the-art technology. Nevertheless,
risks to users, property, and the environment can arise when the device is used carelessly or
improperly.
The manufacturer has determined residual dangers emanating from the device
• if the device is operated by insufficiently trained personnel.
• if the device is not operated according to its proper use.
Appropriate warnings in this manual serve to make the user alert to these residual dangers.
2.5.1 General hazards
Pay attention to the following safety notices:
DANGER
Death or serious injuries by use in explosive environments.
• Do not store or operate the device in explosive environments.
• Provide sufficient ventilation and make sure to directly withdraw fumes
WARNING
Death or serious burns by flammable vapors, flames and sparks.
• Remove all sources of flammable vapors, flames and sparks
• Do not store flammable chemicals in the vicinity of the device
NOTICE
Risk of device damage by liquids or mechanical shocks.
• Do not spill liquids over the device or its components
• Do not move the device when it is loaded with sample liquid
• Do not drop the device or its components
• Keep external vibrations away from the device
• Safely attach the device to the bench in earthquake prone regions
• Do not operate the device without the safety shield installed
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2 Safety
NOTICE
Risk of device damage by wrong mains supply.
• External mains supply must meet the voltage given on the type plate
• Check for sufficient grounding
C-650 Operation Manual, Version B
2.5.2 Warning labels on housing and assemblies
The following warning sticker(s) can be found on the housing or assemblies of the C-650:
Symbol
Meaning Location
Hot item, hot surface Sticker / label, located at the heating block
2.5.3 Personal protective equipment
Always wear personal protective equipment such as protective eye goggles, protective clothing
and gloves. The personal protective equipment must meet all requirements of the supplementary
data sheets for the chemicals used.
WARNING
Serious chemical burns by corrosives.
• Observe supplementary data sheets of all used chemicals.
• Always wear protective goggles.
• Always wear protective gloves.
• Always wear protective clothes.
2.6 General safety rules
2.6.1 Responsibility of the operator
The head of laboratory is responsible for training his personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents which
might occur during operation of the device. Legal regulations, such as local, state and federal
laws applying to the device must be strictly followed.
2.6.2 Duty of maintenance and care
The operator is responsible for ensuring that the device is operated in proper condition only, and
that maintenance, service, and repair jobs are performed with care and on schedule, and by
authorized personnel only.
2.6.3 Spare parts to be used
Use only genuine consumables and genuine spare parts for maintenance to assure good system
performance and reliability. Any modifications to the spare parts used are only allowed with the
prior written permission of the manufacturer.
2.6.4 Modifications
10
Modifications to the device are only permitted after prior consultation with and with the written
approval of the manufacturer. Modifications and upgrades shall only be carried out by an authorized BUCHI technical engineer. The manufacturer will decline any claim resulting from unauthorized modifications.
2 Safety
C-650 Operation Manual, Version B
3 Technical data
This chapter introduces the device specifications. It contains the scope of delivery, technical
data, requirements and performance data.
3.1 Scope of delivery
Check the scope of delivery according to the order number.
NOTE
For detailed information on the listed products, see www.buchi.com or contact your local dealer.
3.1.1 Standard device
Table 3.1: Standard device
Product Order number
ELS Detector C-650 (230V/50 Hz) 11059105
ELS Detector C-650 (115V/60 Hz) 11059106
3.1.2 Standard accessories
Table 3.2: Standard accessories
Product Order number
C-650 signal cable 11059100
C-650 autozero cable 110 5 916 5
C-650 external signal cable 110 5 92 29
C-650 RS232 cable 110 59 2 75
Gas tubing, 6 mm, 2 m + 1 m 110 5 9 276
Set of fuses (115V) 110 5 9172
Set of fuses (230V) 110 5 9173
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C-650 Operation Manual, Version B
3.1.3 Optional accessories
Table 3.3: Optional accessories
Product Order number
Flow splitter 110 5 9 0 07
3.2 Technical data overview
Table 3:4: Technical data
Dimensions (L×H×D) 250×450×550 mm
Connection voltage 115VAC (±10%)/60Hz/1.8A
Weight 18.5 kg
Overvoltage category II
Pollution degree 2
230VAC (±10%)/50Hz/1.7A
Environmental conditions
Temperature
Altitude
Humidity
For indoor use only
5–40 °C
Up to 2000m above sea level
Maximum relative humidity 80% for temperatures up to
31°C, and then linearly decreasing to 50% at 40°C
Detection High sensitivity photomultiplier
Light source Selected high efficiency blue LED
Temperature range Ambient to 100°C
Gas flow control Manual and computer controlled (power down) nebulization
gas flow and patented auxiliary gas flow
Gas consumption Less than 5l/min
Eluent flow rate 0.1mL/min to 5mL/min
Device control Microprocessor with stand alone manual keypad or PC
control
Operating parameters control Liquid crystal digital panel
Signal drift Less than 2mV/30min
Signal output 0–1V (analog), RS-232 (digital)
12
Inputs Remote Autozero (contact closure and TTL)
Remote Power down Mode (contact closure and TTL)
Power Down Mode General
Standby
Cleaning
Zero control Manual Autozero and remote Autozero
3 Technical data
C-650 Operation Manual, Version B
4 Description of function
This chapter explains the basic principle of the device, shows how it is structured and gives a
functional description of the assemblies.
4.1 Overview over the device
Fig 4.1: Overview over the device
The C-650 is designed to detect compounds in the eluent from Preparative Chromatography. It
is capable of monitoring eluent flow rates from 0.1mL/min to 5mL/min. Evaporative Light-Scattering Detection is a nearly universal technique which can detect any non-volatile analyte. Unlike other types of detection mode such as UV Detection, it is not dependent on the absorption
of radiation and is not affected by the absorption characteristics of the solvent. Thus, solvents
which absorb UV radiation can be used. As the solvent is completely evaporated, a gradient can
be performed to optimize the separation.
The detector is controlled via the keypad and digital LCD display on the front panel or by RS-232.
The analog signal output can be sent to a recorder, an integrator or a data station such as BUCHI
SeparcoreRecord or SepacoreControl Software.
The detector includes a nebulization cell, an evaporation tube and a detection chamber. The
evaporation tube is heated in order to evaporate the solvent.
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C-650 Operation Manual, Version B
4.2 Functional principle
There are three discrete steps in the operation of the detector; nebulization of the eluent, evaporation of the solvent and detection of the compound(s) of interest.
Nebulization --> Evaporation --> Detection
Nebulization involves the conversion of the eluent into a fine aerosol. This aerosol is directed to
an evaporator to vaporize the solvent, then the mist is irradiated by a light source and the scattered light is measured by a photomultiplier; which is related to the concentration of the compound of interest in the sample.
A cross sectional view of the device is presented below.
3
a Nebulization
b Evaporation
Fig 4.2: Cross-sectional view of the detector
4.2.1 Nebulization
The eluent from the chromatograph is nebulized by the inlet gas (typically air or nitrogen). At the
outlet of the nebulizer, the aerosol travels through a chamber. Large droplets in the aerosol are
drawn to a siphon while the fine mist travels to the evaporation tube. The overall design of the
nebulizer is shown in Fig 4.3 and the nebulization chamber is shown in Fig 4.4.
2
1
c Detection
14
The Flash Chromatography Nebulizer has a flow rate of 0.1mL/min –5mL/min and a back pressure of 4bar (1mL/min) by the use of water.
4 Description of function
C-650 Operation Manual, Version B
1
2
3
4
a Liquid inlet
b Coloured seal
Fig 4.3: Design of the nebulizer
Fig 4.4: Glassware chamber
c Ring
d Gas inlet
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4 Description of function
C-650 Operation Manual, Version B
4.2.2 Evaporation of the solvent
A heated tube is used to evaporate the solvent. The exit of the heated tube leads directly into the
detection chamber.
In liquid chromatography, water and organic solvents with low boiling points are typically employed (e.g. CH3OH, CHCl3, CH3CN). A typical mobile phase for a reverse phase separation using Evaporative Light-Scattering Detection might be CH3OH/H2O (60/40) while a typical mobile
phase for normal phase separation might be C6H14/CHCl3 (6 0/40).
If acids, bases and salts are used to modify mobile phase to provide the desired separation, they
should be able to be readily evaporated, sublimed or decomposed into gases in the evaporation
tube. Mobile phase modifiers that are commonly used when an Evaporative Light-Scattering
Detector is employed include NH4OH, (C2H5)3N, NH4 Acetate, NH4 Formate, HCOOH, CH3COOH
and CF3COOH.
4.2.3 Detection
The carrier gas transports the microparticles from the heating tube into the detection chamber
(Fig 4.5).
1
2
3
5
a Photomultiplier
b Detection chamber
4
d Additional gas
e Light trap
c LED
Fig 4.5: Detection chamber
The detector chamber contains a Light Emitting Diode (LED) and a photomultiplier that is positioned at an angle of 100° with respect to the light beam (Fig 4.5). When the carrier gas contains
microparticles, the light is scattered and is detected by the off-axis photomultiplier.
The intensity of the scattered light is a function of the mass of the scattering particles and generally follows an exponential relationship, which is shown in the following equation.
16
I = k m
b
where: I is the intensity of light
m is the mass of the scattering particles
k and b are constants
4 Description of function
C-650 Operation Manual, Version B
A plot of log I versus log m provides a linear response. The values of the constants (k and b) are
dependent on a variety of parameters (e.g. the temperature and the nature of the mobile phase).
An inlet to provide additional gas is located immediately before the detector chamber to provide
a concentric shield for the carrier gas. This serves to eliminate diffusion of the carrier gas and
eliminate contamination of the detection chamber.
4.3 Eluent flow splitting
The C-650 detector is designed to work with flow rates from 0.1 to 5mL/min. In preparative chromatography applications, the flow rate is mostly higher than 5mL/min. The BUCHI preparative
chromatography systems can deliver flow rates up to 250mL/min. For preparative applications,
the eluent flow rate coming out of the chromatography column must be split into 2 different flow
rates:
• One part (usually about 1mL/min) is directed to the C-650 and this part of the sample is
destructed by the evaporation and diffraction process.
• The other part is directed to the fraction collector to collect the detected compounds.
The working principle is shown below:
Flow splitter
≤ 250mL/min
Pumping system
Fig 4.6: Working principle of the flow splitting
UV
Column
Detector
(optional)
≤ 5mL/min
Fraction
Collector
ELSD
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4 Description of function
C-650 Operation Manual, Version B
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