Transcript Evaporative Light Scattering Detector Product Range

Evaporative Light Scattering
Detector Product Range
Introduction
Polymer Laboratories ELSD portfolio includes 2 models, each offering
high sensitivity for a wide range of applications
PL-ELS 1000
• Routine GPC and HPLC using high
boiling point solvents
PL-ELS 2100
• Regular HPLC with low temperature
operation for volatile compounds
Application Areas of
PL’s ELSDs
PL-ELS 1000
GPC analysis
• Ambient
• High Temperature
HPLC of non volatiles
• Lipids
• Sugars
(Microbore LC)
PL-ELS 2100
Low temperature analysis
HPLC of volatiles & semi-volatile
analytes
• Pharmaceuticals
• Nutraceuticals
• Combinatorial libraries
Ambient GPC analysis
SFC
PL-ELS 1000 High
Temperature ELSD
Solvent resistance enclosure
Clear Display of Detector
Output and Exhaust temperature
Status LEDs
Removable handset allows
instrument control both on and
off the unit
PL-ELS 1000 High
Temperature ELSD
PL-ELS 1000
Nebulizer
Gas Inlet
Eluent Inlet
The eluent “droplet” is sheared
from the needle by the gas supply
(cross-flow nebulization)
PL-ELS 1000 Evaporator
A large thermal mass ensures
accurate and constant
temperature control
The chamber is independently
temperature controlled
The PL-ELS 1000 can operate
up to 300°C
PL-ELS 1000 Optics
Light Source
(tungsten halogen
lamp)
Detector
(via fiber optic cable
to Photodiode detector)
Safety Features
Vapour sensors
Independent temperature
sensors
Gas flow safety
Electrical surge protection
CE compliant
Solvent Trap and Waste
Nebulizer waste
To extraction system
Drain from solvent trap
Waste drain
Control features and
Modes of Operation
Modes of operation
• Run
– Instrument is fully
operational
• Standby
– Power on, instrument
parameters can be
modified
• Sleep
– Instrument shut down
• Gas Save
– Heaters at operational
temperature
– Gas flow rate and heaters at operational
levels
– Gas flow set at zero, lamp and
heaters off
– Gas flow closed, lamp and heaters
off
– Gas flow at low flow (0.1 SLM)
Control features and
Modes of Operation
Control features
• Control parameters stored as
method.
– 10 locally
– unlimited via software
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System automation
Instrument diagnostics
Operational log
Computer software
Removable handset
System performance testing
PC Control Software and
System Performance Testing
Runs a series of diagnostic checks on the
detector
When used in conjunction with the log
can be used to diagnose errors.
Can be used
performance
to
OQ, IQ and PQ feature
validate
detector
Computer Interface
Polymer Additive Analysis
Most additives are non-volatile and do not possess a UV chromophore. The and
universality and high temperature range of the PL-ELS 1000 provides a
sensitivity detection technique.
Columns : 2 x PLgel 5um 50Å
Eluent :
THF + 0.1%
diethanolamine
Flow rate : 1.0ml/min
100
Response
Chimasorb 944
Irgafos 168
Irganox 1010
0
Tinuvin 622
Tinuvin 770
Tinuvin 327
-100
6
minutes
5
20
20
Minutes
Ciba6.005
Ciba5.006
Ciba5.007
Ciba6.002
Ciba6.004
Ciba5.004
Separation of PEG Using GPEC
The PL-ELS 1000 can be operated at high temperature for polymer analysis,
such as GPEC.
Samples: Narrow polyethylene glycol standards
(Mp 600 and 1470)
Columns: Zorbax 300 SB-C18 5µm, 150x4.6mm
Eluent: ACN: Water
Flow rate: 0.5mL/min
Detector: PL-ELS 1000
Evap 140°C, neb 100°C, gas flow 0.5SLM
Benefits of the PL-ELS 1000
Operating Temperature range from 40 to 300°C
Extremely low dispersion for high resolution
separations
Highly Sensitive and Stable
High eluent flow rates, up to 3ml/min
Low gas consumption
Compatible with High Temperature GPC
Remote control
Easy to use software
Extremely small footprint, stackable
PL-ELS 2100
• Compact, modern design
• Flat top
• Small footprint, stackable
Display
Keypad
• Operation via control panel
and simple keypad
• Column connection at front
of detector
• One exhaust tube at rear,
one liquid waste port at front
Column
Connection
Liquid
Waste
Nebulization
• Eluent flow mixed with N2/Air
• Concentric nebulizer gives efficient
nebulization, stable droplet plume,
uniform droplet size
• Narrower cone of spray plume allows
a smaller nebulizer chamber, which
minimizes band broadening
• Better recovery of semi-volatile
solutes
compared
to
cross-flow
nebulizer
• Easier to align, reproducible from one
detector to another
• Temperature independently controlled
Evaporation
• Solvent removed by heating
•Temperature independently
controlled
• PL-ELS 2100 has an additional gas
input that aids evaporation (patent
pending)
• Small volume evaporator
• Fast thermal equilibration
• Diffuser reduces turbulence inside
evaporator tube which minimizes
band broadening (patented)
Detection
• Blue LED light source (480nm)
• Intensity controllable by user
• Photomultiplier detector tuned to same
wavelength for increased sensitivity
• Feedback control for light source provides
constant output
• Detector mounted directly onto the optics
which eliminates stray light loss and
increases sensitivity
• Reduced volume in the optics chamber,
minimizes band broadening
• Digital gain control to optimize full scale
sensitivity
• Digital signal smoothing to optimize S/N ratio
Digital Signal Processing
• Digital Signal functions are accessed via the down arrow key
in main menu screen
• Parameter Screen allows you to change
- PMT output or gain (1-250)
- Smoothing (1-50)
- LED intensity (0-100)
Simple Operation
Two modes of operation :
STANDBY
• Power on
• LED off
• Heaters off
• Gas at minimum flow rate (1.2 L/min)
- Gas shuts off after 15 minutes
RUN
• Power on
• LED on
• Temperatures and gas flow controlled to set
values
Operating the PL-ELS 2100: Onboard
Instrument Control
Mode
Current method
Actual values of
set parameters
Detector
output
Status
Interactive menu bar
Keypad
PL-ELS 2100 Control Software
 Select mode of operation
 Control parameters
 Evaporator & Nebulizer temp
 Gas flow (0-3.25 L/min)
 Monitor output
 Gain setting (0.1-250)
 Signal smoothing (0-5)
• Log instrument conditions over time
• Load / Edit methods
- 10 programmable methods
PL-ELS 2100 Control Software
• Supplied as standard with the PL-ELS 2100
• Select 1 of 10 different temperature programs according
to analysis
• Also available as a Software Development Kit for third
party system integration
• To use the control software simply connect the PL-ELS
2100 to a PC via a serial connection (RS232) on selectable
COM port
• Where no serial port is available, a USB serial connector
can be used
Method Manager Software
• Used when the instrument is to be controlled via the onboard
instrument control (rather than software control)
• This is a simple software utility designed to set up, edit and
log defined methods which can then be downloaded to the
PL-ELS 2100
• Method Manager Software supplied as standard with the
PL-ELS 2100
• To use this software utility, simply connect the PL-ELS 2100 to
a PC via a serial connection (RS232)
PL-ELS 2100: Routine Operation
• When running with the “XXX” method, the User has complete
flexibility to change parameters via the PL-ELS 2100 keypad
and display (e.g. for method development)
• Once standard methods for operation of the PL-ELS 2100
have been established, these can be stored using the PL-ELS
2100 Method Manager software utility and downloaded to the
unit
• These downloaded parameters are stored as numbered
methods (1-10) and cannot be edited through the keypad, only
by running the PL-ELS 2100 Method Manager software
A New Approach to ELS Detection
• Operating conditions of the PL-ELS 1000 is based on
the properties of the eluent (e.g. high boiling point
solvents require high evaporator temperatures)
• However, the PL-ELS 2100 operating conditions are
determined by the properties of the analyte (e.g. semivolatile or non-volatile)
•The PL-ELS 2100 can evaporate water at ambient
temperature, unlike the PL-ELS 1000.
Manipulating the PL-ELS 2100
Parameters
FOR NON-VOLATILE SOLUTES
• Nebulizer and evaporator can run hot to increase signal to
noise ratio
• Gas flow is set as low as possible to maximize signal
FOR RELATIVELY VOLATILE SOLUTES
• Nebulizer and evaporator run cold to increase signal
• Gas flow is increased to control baseline noise
Volatile Applications: Effect of Changing
Evaporator Temp
Samples:
1. Acetanilide, 2. Indapamide, 3. Ibuprofen,
4. Dibutylphthalate
Column:
C18 5µm, 150x4.6mm
Eluent A:
0.1% TFA in Water
Eluent B:
0.1% TFA in ACN
Gradient:
60-90%B in 5 mins
Flow Rate:
1.0mL/min
Detector:
PL-ELS 2100 (neb and evap set at the same
temperature, gas 1.8 L/min)
Note: peak 2 is non-volatile, peaks 1, 3, 4 are relatively volatile
Volatile Applications: Effect of Changing
Evaporator Temp
• At high temperature peak 2 has better S/N but peaks 1,3,4 are not detected
• At 30°C all four peaks are detected
Environmental
Application:Herbicides
Sample:
Mixture of 10 Phenylurea herbicides
Column:
C18 5µm, 250x4.6mm
Eluent A:
Water
Eluent B:
Acetonitrile
Gradient:
10-80%B in 40 mins
Flow Rate:
0.7ml/min
Inj Vol:
20µl
Detector:
PL-ELS 2100 (neb=25°C, evap & gas flow
varied)
Environmental Application: Herbicides
Non-Volatile Applications:
PEG 400 Separation
Sample:
PEG 400
Column:
PLRP-S 100Å 5µm, 150x4.6mm
Eluent A:
Water
Eluent B:
ACN
Gradient:
10-30% B in 12 mins
Flow Rate:
1.0mL/min
Inj Vol:
10µl
PEG 400: Effect of Changing
Temperature
Higher temperatures increase S/N, no risk of loss due to
evaporation
Evap 90°C
Neb 90°C
Gas 1.6 L/min
Evap 30°C
Neb 30°C
Gas 1.6 L/min
PEG 400: Effect of Changing Gas Flow
Sensitivity is improved as gas flow is reduced
Evap 70°C
Neb 50°C
Gas 1.2 L/min
Evap 70°C
Neb 50°C
Gas 2.4 L/min
Non-Volatile Application:
Triglycerides in Natural Oils
Sample:
2mg/ml Starflower Oil
Column:
C18 5µm, 250x4.6mm
Eluent A:
ACN
Eluent B:
DCM
Gradient:
30-50% B in 40 mins; 50-90% in 2 mins,
hold for 3mins
Flow Rate:
1.0ml/min
Inj Vol:
20µl
Detector:
PL-ELS 2100 (neb=40°C, evap=70°C,
gas=1.4 L/min)
Advantages of ELSD: Uniformity of
Response
Comparison of UV and ELS traces show that ELSD
allows for a more uniform response than UV
detection
Column: PLRP-S 100Å 5µm, 150 x4.6mm
Eluent A: 50% 0.1% TFA in Water : 50% 0.1% TFA in ACN
Flow Rate: 1.0ml/min
Inj Vol:
10µl
Detector: PL-ELS 2100 (neb=30°C, evap=30°C,
gas=1.4 L/min)
UV-VIS @ 280nm
Comparing PL-ELS 1000 & 2100
response
PL-ELS 2100 gives better mass response due to lower temperature
operation
80°C
30°C
Response
PL-ELS 2100: Fast Gradient, Fast Flow
Rate Capability
• Stable baseline throughout the gradient
• PL-ELS 2100 can operate in 100% up to 5ml/min
13.0
2ml/min
11.2
3ml/min
9.4
4ml/min
7.6
5ml/min
5.8
4.0
0.0
0.6
1.2
min
1.8
2.4
Minutes
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channel 4)
channel 4)
channel 4)
channel 4)
3.0
PL-ELS 2100:
DMSO Transparency
Sample:
Pharmaceutical Mixture in DMSO
Column:
C8 5µm, 50x4.6mm
Eluent A:
Water
Eluent B:
Acetonitrile
Gradient:
5-100% B in 5 mins
Flow Rate:
1.0ml/min
Inj Vol:
20µl
Detector:
PL-ELS 2100 (neb=25°C, evap & gas flow
varied)
Ideal for High Throughput Screening
Loss of volatile species occurs as temperature is increased
Ideal for High Throughput Screening
•The design of the PL-ELS 2100 makes it transparent to DMSO at 25-30°C
• Great potential in the High Throughput Combichem market
• Unique to the PL-ELS 2100 due to its use of evaporation gas
PL-ELS 2100: neb=25°C, evap=30°C
Benefits of ELSD
Universal detector: independent
properties of the solute
of
the
optical
Compatible with gradient elution
Ideal for fast gradient elution:- no solvent front.
Removes the need for derivatization
Compatible with chromatographic techniques such as
MS and SFC
Wide application area
Additional Benefits of the
PL-ELS 2100
Operation in 100% water at 25°C
DMSO transparency at ambient temperature
Extremely low dispersion for high resolution separations
(e.g. SFC)
High sensitivity to volatile compounds
Compatible with eluent flow rates, up to 5ml/min
Rapid thermal equilibration
Easy to use
Extremely small footprint, stackable