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Installation,
Mark Sinnott & Alex UcciJune 28, 2018
Agilent Restricted1
and Maintenance of Capillary Gas Chromatography Columns
"It's not what your column can
do for you, but what you can
do for your column"
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Column Installation Procedure
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"Getting off to a good start"
• Install the column
• Leak and installation check
• Column conditioning
• Setting linear velocity or flow rate
• Bleed profile
• Test mix
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Column InstallationWhat type of ferrule should I use?
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Graphite / Polyimide blend capillary ferrules
Unfortunately … leak following normal temperature program runs
Studies show the leaking continues with use of the ferrules -
Not just after the first one or two runs
Frequent re-tightening of the fitting is needed to maintain a leak-free seal – and system performance and productivity
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Better Connections: Self Tightening Column Nuts
Designed for use with short graphite/polyimide blend ferrules –both at the inlet and the MS interface – so only one type of ferrule needed for both ends of the column!
Short ferrule exposes more thread of the fitting for better sealing
For mass spec transfer line
P/N 5190-6194
For inlet or detector
P/N 5190-5233
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How do Self Tightening Column Nuts work?
• Ease of use – install in dark, small space in GC oven without wrenches
• Wing design for finger tight installation with graphite/polyimide blend ferrules
• No tools dramatically reduces force preventing over tightening or damage
• Robust stainless steel construction
Plus….
• Novel spring driven piston design that
continuously presses against the ferrule
to maintain a leak-free fitting
even when the ferrule shrinks during temperature program!
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Benefit of Self-Tightening Column Nuts
Without retightening, the baseline remains flat after 400 runs with no indication of leaks when using the Self tightening Column Nut
Ref. Tech note: 5991-3612EN
Take you from this….
…. to this!
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Column InstallationMeasuring the right distance
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White out Septa
Extra septa
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Cutting The Column
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Gently scribe through the polyimide coating.
Do not attempt to cut the glass.
Recommended tools:Diamond or carbide tipped pencil; or sapphire cleaving tool, ceramic waferOcular
Do not use:Scissors, file, etc.
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Example of a Bad Cut
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A poor cut will definitely get
you off to a bad start
• Active sites created
• Poor peak shape/tailing
= UNHAPPY
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Examples of Column Cuts
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Good
Bad
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Column Installation
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How tight is tight?
Over-tightened Ferrule
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Column InstallationLeak Check
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DO NOT USE SNOOP
Electronic leak detector
IPA/Water
Inject a non-retained peak G3388B Leak Detector
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Leak and Installation CheckInject a non-retained compound vs DB-1
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The peak should be sharp and symmetrical
Detector Compound
FID Methane or Butane
ECD MeCl2 (headspace or diluted)
NPD CH3CN-acetonitrile (headspace or diluted)
TCD Air
MS Air or Butane
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Non-Retained Peak Shapes
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Good Installation Improper Installation orInjector Leak
Check for: -Too low of a split ratio
-Injector or septum leak
-Liner problem:
(broken, leaking, misplaced)
-Column position in injector and detector
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Calculating Linear Velocity
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Inject a non-retained compound and obtain the retention time:
µ is dependent on column temperature, but
is independent of column dimensions
µ=to
Lµ = Average linear
velocity (cm/sec)L = Column length (cm)to = Retention time (sec)
He 20-40 cm/secH2 35-55 cm/sec
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Calculating Flow Rate
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Inject a non-retained compound and obtain the retention time:
F is dependent on column temperature
Measuring flow with a flow meter is often inaccurate
F = Flow rate (mL/min)
r = Column radius (cm)
L = Column length (cm)
to= Retention time (min)
=Fr2L
to
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Column Conditioning
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System must be leak free before conditioning column
Heat the column to the lower of:
Isothermal maximum temperature OR
20° to 30°C above highest operation temperature
Temperature programming is not necessary
Stop conditioning when the stable baseline is obtained:
1 to 2 hours in most cases
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Contamination from French Fry Grease
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Column: DB-5ms, 30m x 0.25mm, 0.25um
Carrier: H2, 60 cm/sec, constant flow
Injector: split 1:20, 250C
Detector: FID, 320C, N2 makeup gas
Oven: 40C for 0.75 min, 40-325C at 20C/min, 325C for 30 min
Red: McFrench Fry
Blue: system blank
Procedure:
(1) Held french fry for 5 seconds.
(2) Fingertip was wiped with paper towel to remove as much of the offending material as possible.
(3) Lightly touched the part of the column sticking up above the ferrule.
(4) Installed column into injector.
(5) Set oven temperature to 40C.
(6) Started oven temperature program as soon as oven reached 40C.
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Generating a Bleed Profile
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Temperature program the column without an injection*
*DB-1 30m x .32mm I.D., .25µm
Temperature program // 40°C, hold 1 min // 20°/min to 320°C, hold 10 min.
Time (min.)0 5 10 15 20 25
6000
7000
8000
9000
1.0e4
1.1e4
1.2e4
1.3e4
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Column Performance Summary
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Chromatographic Performance
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Test Mixture Components
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Compounds
Hydrocarbons
FAME’s, PAH’s
Alcohols
Acids
Bases
Purpose
Efficiency
Retention
Retention
Activity
Acidic Character
Basic Character
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Own Test Mixture
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• More specific to your application
• Selective detectors
• Concentrations specific to your application
• Use same instrument conditions
• Easiest to simply inject a calibration standard
• Store for future measure of column performance
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An Ounce of Prevention......
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Common Causes of Column Performance Degradation
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• Physical damage to the polyimide coating
• Thermal damage
• Oxidation (O2 damage)
• Chemical damage by samples
• Contamination
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Physical Damage to The Polyimide Coating
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• The smaller the tubing diameter, the more flexible it is.
• Avoid scratches and abrasions
• Immediate breakage does not always occur upon physical damage
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Thermal Damage
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Degradation of the stationary phase is increased at higher temperatures. Breakage along the polymer backbone.
Dimethylpolysiloxane
CH3 CH3CH3
CH3 CH3CH3
O
Si SiSi
OOO
• Rapid degradation of the stationary
phase caused by excessively high
temperatures
Isothermal limit = Indefinite time
Programmed limit = 5-10 minutes
• Temporary "column failure" below lower
temperature limit
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Thermal Damage
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•Disconnect column from detector
•“Bake out” overnight at isothermal limit
•Remove 10-15 cm from column end
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Oxidation (O2 Damage)
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Oxygen in the carrier gas rapidly degrades the stationary phase. The damage is accelerated at higher temperatures. Damage along the polymer backbone is irreversible.
Dimethylpolysiloxane
CH3 CH3CH3
CH3 CH3CH3
OSi SiSi
OOO
O2
~ 5% O2
Decreased retention
Re
du
ce
d r
esp
on
se
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How to Prevent Column Damage by Oxygen
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• High quality carrier gas (4 nine's or greater)
• Leak free injector and carrier lines
Change septa
Maintain gas regulator fittings
• Appropriate impurity traps
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Configurations for Carrier Gas Purifiers
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IndicatingMoisture Trap
High CapacityOxygen Trap
Indicating Oxygen Trap
Hydrocarbon
Indicating Moisture
Indicating Oxygen
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Chemical Damage
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Bonded and cross-linked columns have excellent chemical
resistance except for inorganic acids and bases
Chemical damage will be evident by excessive bleed, lack
of inertness or loss of resolution/retention.
HCl NH3 KOH NaOH
H2SO4 H3PO4 HF etc.
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Chemical DamageWhat To Do If It Happens
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• Remove 1/2 - 1 meter
from the front of the
columns
• Severe cases may
require removal of up to 5
meters
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What is Normal Column Bleed
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Normal background signal generated by the
elution of normal degradation products of the
column stationary phase
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Column Bleed is Influenced by:
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06000
7000
8000
9000
1.0e4
1.1e4
1.2e4
1.3e4
5 10 15 20 25Time (min.)
24 pA / 260°C
DB-624 30M x .53mm I.D., 3.0µm
12 pA / 320°C
DB-1 30m x .32mm I.D., .25µm
Phase type
Temperature
Column dimensions
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Mass Spectrum of Phenylmethylpolysiloxane Column Bleed (Normal Background)
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Mass spectral library search is not always accurate
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What is a Bleed Problem?
An abnormal elevated baseline at high temperature
IT IS NOT
A high baseline at low temperature
Wandering or drifting baseline at any temperature
Discrete peaks
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Column Contamination
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•Fouling of GC and column by contaminants
•Mimics nearly every chromatographic problems
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Symptoms of Contamination
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• Poor peak shape
• Loss of separation (resolution)
• Changes in retention
• Reduced peak size
• Baseline disturbances (semi-volatiles only)
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Typical Samples That Contain a Large Amount of Residues
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Biological (Blood, Urine, Tissue, Plants)
Soils Foods
Waste Water Sludges
All samples contain residues!! (even standards!)
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Other Sources of Contamination
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•Septum and ferrule particles
•Gas and trap impurities
•Unknown sources (vials, syringes,etc.)
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Non-Volatile Residues
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Any portion of the sample that does not elute from the
column or remains in the injector.
Semi-Volatile Residues
Any portion of the sample that elutes from the column after
the current chromatographic run.
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Methods to Minimize Non-Volatile Residue Problems
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• Sample cleanup
• Packed injection port liners
• Guard columns
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Agilent Restricted45
Agilent Bond Elut Sample Clean-Up Products
Solid Phase Extraction
Cartridges and Plates
Filtration Cartridges
and Plates
Captiva EMR Lipid
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Guard Column or Retention Gap
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The guard column is 3 - 5 meters of deactivated fused silica tubing with the same diameter as the analytical column. It is connected with a zero dead volume union.
INJECTOR DETECTOR
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Non-Volatile ContaminationWhat To Do If It Happens
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•Do not “bake out” the column
•Front End Maintenance
clean or change the injector liner
clean the injector
cut off 1/2 -1 meter of the front of the column
•Turn the column around
•Solvent rinse the column (see appendix)
•Cut the column in half
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Semi-Volatile ContaminationWhat To Do If It Happens
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• “bake out” the column
• Limit to 1-2 hours
• Longer times may polymerize some
contamination and reduces column life
• Solvent rinse the column
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Column Storage
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•Place septa over the ends
•Return to column box
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The New Agilent Intuvo 9000 GC System
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Common frustrations with GC
• Measuring column length correctly
• Cutting your column correctly
• How tight it too tight?
• Clipping columns to deal with active sites, then updating
retention times
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Common Care and Maintenance Scheme for GC Columns
1. Cut off 6”-1ft of the inlet end of the column.
2. Bake out the column for no more than 2 hours.
3. Cut off more column. (repeat as necessary)
Guard Column
Intuvo…
Change the guard chip
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Innovating the GC Flow Path
Click-and-run
direct
connections
To detector
To detector
Conventional
flow path
Intuvo
flow path
Inlet Inlet
Guard chip
Intuvo planar
column
Gold seal
Nuts and ferrules
Classic capillary
column
Flow
chip
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Easier and faster maintenance with Intuvo
• No more ferrules
• Direct face seal connections
• Audible and tactile click lets
you know connection is made
• Less unplanned downtime
• Fewer batch reruns and
precious samples lost
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No More
- measuring
- over-tightening
- trimming
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A New Portfolio of GC Consumables
UI Inlet LinersGuard Chip
No-trim
column
Intuvo
Flow
Chips
Smart Keys
Tools &
Accessories
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No More:
- Measuring
- Over-tightening
- Trimming
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Tips to Assure a Good Column Installation
1. Finger tighten until only 1 thread on each of the two nuts is showing.
If more than 1 thread is showing, wiggle or re-position the column into place to further finger tighten the nuts to 1 thread.
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Tips to Assure a Good Column Installation
2. Check that the small integrated column nuts on the column are in form fitted place on the heater in the instrument.
3. Click and Run!!
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Smart Key Technology
• Smart chip tells your Intuvo
what you have
• Sets temperature limits for
you
• Keep track of performance
with read/writeable Smart Key
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Where Does it Get Dirty?
Here
Here
Here
Here
Here
Here
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Not the Column!Agilent Restricted
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New Autonomous Leak Checking
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Agilent Intuvo 9000 Videos:
The Agilent Intuvo 9000 GC System – Environmental Science Corporation (ESC)
Discover higher GC productivity with the Agilent Intuvo 9000 GC system.
Playing Time: 4:00
The Agilent Intuvo 9000 GC System Story
Learn more about the Agilent Intuvo 9000 GC System
Playing Time: 2:21
The Agilent Intuvo 9000 GC System: Return on Investment. Return on Innovation
A testimonial regarding the return on investment on the Agilent Intuvo 9000 GC System
Playing Time: 4:17
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Always Remember to:
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• Start with a good installation
• Maintain an oxygen free system
• Avoid physical, thermal, and
chemical damage
• Take steps to prevent
contamination
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Contact Agilent Chemistries and Supplies Technical Support
1-800-227-9770 Option 3, Option 3:
Option 1 for GC/GCMS Columns and Supplies
Option 2 for LC/LCMS Columns and Supplies
Option 3 for Sample Preparation, Filtration and QuEChERS
Option 4 for Spectroscopy Supplies
Available in the USA 8-5 all time zones
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Appendix
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Column Rinse Kit
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1/16" flexible teflon line to regulated pressure source
Beaker for solvent collection
Capillary column
Special connectorand ferrule
Flexible teflontubing
Special adapter
Cap
Vial
Capillary column
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• One of Agilent’s newest products with a 2 in 1 benefit of removing proteins and
lipids
• Simple pass-through format
• Solvent-retention frit in 1 mL cartridge/96-well plate format for in well protein
precipitation (in situ)
• Unique cartridge/well construction minimizes clogging – and ensures protein
and lipid removal (no cloudy samples)
• 3 and 6 mL cartridge format for larger samples
• Do not contain solvent retain frit which allow for gravity flow
• Protein precipitation performed offline (QUECHERS, etc.)
• Unique cartridge/well construction minimizes clogging – and ensures protein and
lipid removal (no cloudy samples)
• High analyte recoveries
• Effective use will reduce ion suppression, increase analyte sensitivity, and
detection, and extend the lifetime of your analytical column
Captiva EMR-Lipid
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Enhanced Matrix Removal: EMR-Lipid
Free Fatty Acids
Phospholipids
Triglycerides
EMR-Lipid sorbent technology effectively traps lipids through two mechanisms:
✓ Size exclusion – Unbranched hydrocarbon chains (lipids) enter the sorbent; bulky analytes do not
✓ Sorbent chemistry – Lipid chains that enter the sorbent are trapped by hydrophobic interactions
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Protein Precipitation vs. Captiva EMR-Lipid RSD and Peak Area
RSD < 3%RSD > 25%
Protein PrecipitationCaptiva EMR-Lipid
Lipids cause reproducibility problems resulting in high RSD values
Using Captiva EMR-Lipid → low RSD values and higher peak areas
Higher peak area due to less ion suppression → can lead to lower detection limits
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