Agilent GPC Solutions · Agilent PL-GPC 220 Fully integrated, ... (Rg) Viscosity detector detector...
Transcript of Agilent GPC Solutions · Agilent PL-GPC 220 Fully integrated, ... (Rg) Viscosity detector detector...
Agilent GPC Solutions
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Agilent PL-GPC 220
Fully integrated, high-temperature dedicated GPC system
• Operates from ambient to 220 ºC, covering all GPC applications
• All sample carrying components heated to required temperature
– Eliminates sample precipitation
• High temperature detectors housed
inside the oven
– Refractive Index (Included)
– Viscometer (Optional)
– Light Scattering (Optional)
• Powered by Agilent 1260 pump
– Includes degasser
• Dedicated control software
– PL-GPC 220 Control
• Cirrus GPC software for data analysis
Accurately controlled column
oven with integrated injection
system, columns and detector(s)
Temperature controlled
solvent delivery module
with solvent reservoirs,
Agilent pump and degasser
Dual temperature
zone autosampler
prevents sample
degradation
PL-GPC 220
High precision
Agilent pump
ensures
reproducible
results even
in viscous
solvents
Sample is heated from injection to waste to maintain sample solubility & stability
Solvent Delivery
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0
50
0 15
The flow rate reproducibility has been verified
by experimentation and reflect the total system
performance. The value quoted has been
calculated from analyses performed in THF at
40°C and TCB at 160°C
Type Specification
Hydraulic system Dual piston in series pump with proprietary servo-controlled
variable stroke drive, floating pistons
Flow precision ≤0.07 % RSD, or ≤ 0.02 min SD whatever is greater, based on
retention time at constant room temperature
Flow accuracy ± 1 % or 10 μL/min whatever is greater
Built-in Degasser 4-channel degasser
Injection point Hot Zone
Warm Zone
50
100
200
Te
mp
era
ture
(C
)
-20 -10 0 10 20
Vial Position
Carousel Motion
Injection Point
Agitated
PL-GPC 220 Autosampler
Dual Zone Autosampler
40 vial position carousel
2 ml glass vials with crimped aluminum caps
Sample can be slowly stirred prior to injection
Two zone heating, minimized risk of sample degradation
PL-GPC 220 Autosampler
Effect of Autosampler Temperature
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Analysis of commercial polypropylene samples held in carousel for prolonged
period of time
Without dual zone heating, significant degradation of the sample can occur
over extended periods in the autosampler
By controlling the temperature profile, degradation can be minimised
Oven To Injection
Valve Injection system
Vial is transported up to the column oven
Vial equilibration time in the oven is
programmable
Excess solution returned to vial
No risk that the polymer will precipitate
out of solution and cause a system
blockage
Injection precision RSD <1% with no
cross contamination
PL-GPC 220 Autosampler
Hot
Cold
Columns
Pump
Injection System
Electrically actuated injection valve
Flushed fixed loop injection Interchangeable loop volume, 5 - 500 µl
Loop and valve in oven Eliminates sample precipitation and blockages
No contact between solvent
and syringe
Avoids sample carryover and contamination of syringe
Extends lifetime and reduces maintenance required
Jul14.011 Jul14.007 Jul14.008 Jul14.009 Jul14.010 Jul14.006 Jul14.012
Response
Minutes
0
30
5 8 11 14 17 20 23 26 29 32
Djul14.012 Djul14.006 Djul14.007 Djul14.008 Djul14.009 Djul14.010 Djul14.011 Djul14.005
dw
/dlo
gM
logM
0.0
0.1
0.2
0.3
0.4
0.5
2 3 4 5 6 7
Overlaid raw data
chromatograms
Overlaid molecular weight
distributions
Repeatability of GPC (polyethylene)
Injection No. Mn Mw Peak Area
1 17,289 76,818 333851
2 16,988 77,434 335496
3 17,248 77,514 332616
4 17,251 77,052 335635
5 17,348 76,520 334212
6 17,487 77,728 333511
7 16,898 77,578 335642
8 17,457 77,288 334923
Mean 17,302 77,241 334485
s.d. 220 687 1048
% variance 1.3 0.5 0.3
Column Oven
Multi-heater (x8), forced air oven
Rack mounted GPC columns
Up to 6 x 30cm columns
Injection valve
DRI detector
Vapour sensor
High temperature, precise column oven
Easy access for simple column change and routine maintenance
Fully enclosed system, complete outer surface of unit at safe temperature
Temperature range of ambient to 220 °C
Temperature stability: ≤0.05 °C/hour
Space for integrated Viscometer and
Dual Angle Light Scattering detectors
DRI
Viscometer
Light scattering detector
Injection valve, columns and up to three detector modules
through to waste can be heated to 220 °C in the same oven
• Critical to maintain sample solubility throughout the analysis
• Only available system on market that is fully integrated
Temperature stability is key, and the PL-GPC 220 is maintained
at ≤0.05 °C/hour
Triple detection within the PL-GPC 220
Open oven environment
allows easy access
Built in vapour sensors
maintain high safety levels for
the operator
Maintaining sample solubility to the end
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Solvent Delivery Module
Heated Transfer Line from oven to waste bottle
Enclosed system to prevent solvent fumes escaping
Full extraction from rear of unit
Solvent leak sensor with automatic system shut-down
Safety Features
2009 Agilent Innovations Seminar
Solvent Delivery Module
Heated Transfer Line from oven to waste bottle
Enclosed system to prevent solvent fumes escaping
Full extraction from rear of unit
Solvent leak sensor with automatic system shut-down
Dual Angle Light Scattering Detector
detector response directly proportional to weight average
molecular weight (Mw) of the polymer
no column calibration required
scattered light intensity measured at more than one angle
permits determination of radius of gyration (Rg)
Viscosity detector
detector response proportional to the intrinsic viscosity [ ] of
the polymer
generate molecular weight values for a variety of polymer
types via Universal Calibration approach
permits determination of branching in polymers
Molecular weight sensitive detectors for GPC
LS 90•
LS 15°
Visc
DRI
Retention time / min
Polystyrene standards
Mp = 520,000 and
Mp = 9,680 g/mol
Retention time / min
LS 90•
LS 15°
Visc
DRI
Polyethylene NBS 1475
(2.29 mg/ml, 200 µl)
Triple detection
Filtration of Samples at High Temperature
Ideally samples for high temperature analysis are prepared with no
filtration step
• Get the full picture of your polymer constituents
• Most accurate way to use advanced detection
However,the presence of insoluble material in polymer solutions for GPC
analysis can cause major problems by blocking the column frits, resulting
in high back-pressure which degrades column performance
• Remove insoluble material before introduction to system
Many commercial polymers contain insoluble fillers such as carbon black
which must be removed from solution prior to analysis
• Remove fillers before introduction to system
However, many crystalline polymers are only soluble at high temperatures
• Filter polymer solutions at high temperature to avoid precipitation
Shaker / Agitator
Thermostated
Sample Blocks
Hand Pipettor
/ filter
Temperature and
Shaker Controls
PL-SP 260 VS Sample Preparation System
High temperature dissolution and filtration of polymer samples
PL-SP 260VS Sample Preparation System
Developed to allow routine, reproducible sample dissolution,
agitation, and filtration at elevated temperatures.
Compatible with a wide range of solvents.
Suitable for hot solvents up to 260 °C including DMF, DMSO,
DMAc, TCB, o-DCB, and m-Cresol.
Filtration of solutions using either stainless steel frit or glass
fibre membrane filters.
Range of filter porosities available, allows filtration of polymers
containing fillers such as carbon black
PL-SP 260VS Hand Pipettor
DISPLACEMENT
BUTTON
SLOT FOR FILTER CARTRIDGE
CLAMPING LEVER
FILTER CARTRIDGE
4 Frit/filters per cartridge
Colour coded to indicate porosity
Clear centre hole for cleaning and for
transfering samples without filtration
A. Sample unfiltered and transferred by pipettor
B. Sample filtered through 1 µm glass fibre membrane
C. Sample filtered through 2 µm Stainless Steel Frit
D. Sample filtered through 0.5 µm Stainless Steel Frit gives
high resistance, and very little carbon is filtered out
A B C D
Filtering Carbon Filled PE
PL-GPC 220 Applications
– Polystyrene
– Polybutylene Terephthalate (PBT)
– Polyethylene (PE)
– Polyethylene High Molecular Weight
– Polyethylene Ultra High Molecular Weight (UHMWPE)
– Ethylene - Vinylacetate copolymers (EVA)
– Poly(ethylene -co - norbornene)
Summary
The PL-GPC 220 and Agilent PL column technology provides unmatched
accuracy, flexibility and performance for HT-GPC
The advanced design of the PL-GPC 220 allows Conventional GPC
coupled with Viscosity and LS detectors to provide a more thorough
characterization of polymers such as polyolefins
Variability in sample preparation procedures can be eliminated by using
the PL-SP 260VS Sample Preparation System, whilst also providing a
unique mechanism for analysing polymer solutions requiring high
temperature sample filtration
Agilent Technologies provides a complete solution for the difficult
analyses demanding High Temperature GPC
Agilent has the portfolio to offer a world leading complete
GPC solution
• GPC Instrumentation
− Including advanced detectors
• GPC Software
• GPC Columns
− Including specialist columns for polyolefins
• GPC Standards
• GPC Expertise
Agilent Technologies Complete GPC Solution
PL-GPC220 Analysis of Commercial Polystyrene
Column: 2x10µm MIXED-B, 300x7.5mm
Flow Rate: 1.0ml/min
Eluent: THF
Temp: 40°C
Polyester/Polyamide Applications
PET
Nylon 6,6
Nylon 6
HFIP is an alternative solve
nt, viscous but low boiling p
oint
Column: 2xPL HFIPgel, 250x4.6mm
Eluent: HFIP + 20mM NaTFAc
Temp: 40°C
Flow Rate: 0.3 ml/min
Detector: DRI
Ethylene - vinyl Acetate Copolymer Samples
Column: 3xPLgel 10µm MIXED-B, 300 x 7.5mm
Eluent: TCB + 0.00125% BHT
Flow Rate: 1.0ml/min
Temp: 160°C
Sample A
Sample B
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