Tecnología microfluidica como base
a las técnicas avanzadas de GCxGC y
LTM
Page 1
19 de Julio de 2012
UNIVERSIDAD DE SALAMANCA
Departamento de Química Analítica, Nutrición y
Bromatología
Marc Gibert
Ingeniería Analítica S.L.
Ingeniería Analítica S.L.
Su Partner Tecnológico en
Integración de periféricos sobre
Equipos Agilent
es
Soluciones para todos los niveles de exigencia
Nivel V • Solución completa con componentes tanto de Agilent como de otros fabricantes.
• Incluye HW,SW,Consumibles y materiales de referencia.
• Se garantiza las especificaciones de la normativa a la que se refiera.
Nivel IV • Incluye HW,SW,consumibles de Agilent probados y soportados por un VAR
• Se transfiere el conocimiento sobre la aplicación.
Nivel III
•Cada sistema sale de fábrica comprobado para cumplir el método regulado que se requiera
•Se desarrolla la documentación especifica requerida y se envía con cada solución.
•SP1 7890-0458 GC/MS Toxicology Screening Analyzer
Nivel II
•Aplicaciones probadas con configuraciones concretas
•Comprobadas con múltiples muestras y bajo varias condiciones
•Se suministra todos los componentes requeridos(HW,SW,C&S,Servicio)
•3876AA – LC/(Q)TOF Forensic/Tox PCDB and Spectrum Library kit
•G1734AA – LC/QQQ Forensic/Tox Dynamic MRM Database Kit
Nivel I • Notas de aplicación descritas de forma detallada y cuya fiabilidad ha sido probada.
Kits aplicación
Notas de aplicación.Metódicas
Analizador Agilent
Channel Partner Analyzer
“Field Solutions”
1. Desarrollo de proyectos “Llave en mano”
-Estudio y desarrollo e implementación de proyectos
-Selección, elección e instalación de equipos y
configuraciones instrumentales
-Desarrollo, Implementación y validación de métodos
analíticos en laboratorio de cliente
-Soporte continuado
-Servicios analíticos avanzados
2. Instrumentación Analítica
GC
GC/MS
HPLC
HPLC/MS
HEAD SPACE
PURGE&TRAP
DESORBCION TERMICA
PIROLISIS
DETECTORES SELECTIVOS SCD,NPD,PFPD, HID, XSD,AED...
GENERADORES DE GASES
TOC
. . . . . . .
3. Soluciones Analíticas
- Aplicación de técnicas modernas a
la solución de problemas específicos
- Analíticas instrumentales con
acoplamientos complejos
4. Consumibles . . . y los 2000 productos y accesorios más
utilizados en analítica instrumental
Soporte a nuestra base instalada con la venta de
consumibles AGILENT así como de los consumibles de
los equipos periféricos acoplados. (Markes, Tedelyne
Tekmar, Oi Analytical, Vici Valco, Pal, Leap
Technologies, CDS, Horizon, Antec, Wheaton,LPP,
Hamilton, SGE...)
Capillary Flow
Technology
-- solves difficult application
problems easily & opens up
many new (and old)
possibilities for GC & GC/MS
IF We Only Had A Technology That Provided Easy,
Reliable Flow Structures In The GC Oven...
It would open up many new (and old) capabilities for GC
– Column connections (connect pre-column)
– Change MSD columns (without venting)
– Backflush (Reverse flow through column)
– Detector splitter (effluent split to two or more detectors)
– Merge flows (2 columns to 1 MSD)
– Deans switch (heart cut select peaks to 2nd column)
– Comprehensive 2-D GC (cut all peaks to 2nd column)
– etc.
Metal
Fittings
Press Fit
Glass
Graphite
Polyimide
Packed columns,
reliable
Low dead volume,
inert, low cost
High temperature
Low initial leakage
Types of Connectors Used In The GC Oven
Not inert, no ferrule
for capillary columns
Difficult to assemble,
comes apart
Sheds active graphite
particles into sample
path
Loosens and leaks
with oven cycling,
solvent tailing
Advantages Limitations
Challenges For Inside the Oven Devices
– Inertness (it is in the sample path)
– Low dead volume (it is in the separation path)
– Leak free (especially with repeated temp cycling)
– Fast thermal response (follow rapid oven ramping)
– High temp tolerance (GC oven can go over 350C)
– Reliable and easy to use
5 Key Developments in Capillary Flow
Technology
Complex flow structures with low thermal mass
Makes metal surfaces as inert as column
Backflushing now possible, change MSD
columns without venting, known column outlet
pressure
Accurately predict flows and pressures
BEFORE installing devices
Easy to use, do not loosen or leak with oven
cycling to 400°C
Manifold
Plates
Deactivation
of Metal
EPC
Calculators
Metal
Ferrules
Capillary Flow Technology- Design
• Photolithographic chemical milling for low dead volume
• Diffusion bond two halves to form a single flow plate
• Small, thin profile provides fast thermal response
• Projection welded connections for leak tight fittings
• Deactivation of all internal surfaces for inertness
… a proprietary Agilent Technology
The Metal Ferrule
Square cut is
not critical
Seal region
Does not loosen (leak) even with thousands of runs to
350C
Does not shed particles
3-Way Splitter With Makeup Effluent Splitter
(3 Way)
Column in
Aux EPC in Det1 out
Det2 out Det3 out
Capillary Flow Technology
Column 1
In
Restrictor 1
out to vent
Plate
Ferrule
Nut
Restrictor 2
or Column 2
Channel
Comparison of New Fitting with Polyimide
Fitting
Polyimide
Fitting
New Fitting
Exposure to polyimide and unpurged annular
spaces is greatly reduced
Ferrule Ejector Hole
Polyimide
FID direct
Capillary Flow fitting
Capillary Flow Technology fittings avoid tailing with
small but well swept dead volume
1.1 1.15 1.2 1.25 1.3
0
1
2
3
4
5
6
Pentane test chromatogram
Fitting Design Minimizes Tailing
Capillary Flow Technology- Capabilities
Detector Splitting
Solvent Bypass
Heart Cutting (Deans Switch)
QuickSwap
Modulation (GCXGC)
Backflush
Capillary Flow Technology Devices
Ultimate Union Ultimate Union
7890 GC
Column
FID
Precolumn
Gas Sampling Valve
7890 GC
Column
FID
Tube to Connector
Tube Connector
Reliable precolumn
connector
Easy valve to capillary
column connector
Tube is 0.25 mm id and
is deactivated
Splitters: Unpurged Tee
1:1 split FPD:uECD
Effluent Splitter
WITHOUT Makeup
Auto-sampler
7890A
GC
Column
0.3 m X 0.25
mm id
30 m X 0.25 mm id X 0.25 um HP-5MS
FPD P
mECD
Simultaneous detection with 2 detectors (but NOT
MSD) Cannot do backflushing
Det 2 OUT
Column IN
Det 1 OUT
SPLITTER VARIABLE de Ingenieria Analitica
para equipos Agilent
flexibiliza el ajuste de respuestas
en la multi-detección simultánea
Claves del SPLITTER VARIABLE:
– Emplea la fiable tecnología de AGILENT como base
– Control integrado en CHEMSTATION como parte de cada método
– Rango completo de SPLITT (0-100:100-0)
– Puede trabajar a RT constantes o a mínimo caudal
– Programable a lo largo del análisis
– Reproducibilidad y estabilidad del SPLITT a lo largo del análisis y entre diferentes análisis
– Adaptable a cualquier detector y método de trabajo
– Permite la realización de Backflush
– Permite el cambio de columna sin detener los detectores
SPLITTER VARIABLE
DET #: FID, TCD, PFPD, SCD, NPD, MSD, AED, Sniffer...
Auto-sampler
6890 o 7890
GC
Columna DET 2
DET 1 AUX EPCs
SPLITTER VARIABLE
QuickSwap
MSD Transferline Auto-sampler
7890A
GC
Column
AUX EPC
4 psig
171 mm X
0.121 mm id
restrictor
5975C Inert
MSD
Change MSD columns without venting
Backflush heavy components out split vent
QuickSwap MSD Interface
Remove column w/o venting
– Air & H2O blocked
Safe disconnection of column
from inlet for inlet maintenance
– Reversed flow through column
during inlet maintenance
Backflushing
– Removes heavies from column
Maintain constant flow to MSD
(flow rates exceeding 2 mL/min require an MSD with Performance Turbo)
MSD
Transfer
Line
Aux EPC In
Column Effluent
Backflush with QuickSwap
S/S Inlet
QuickSwap
Column
1 psi
45 psi
MSD
Aux EPC Split Vent Trap
During GC Run
After GC Run
S/S Inlet
QuickSwap
Column
25 psi
4 psi
MSD
Aux EPC Split Vent Trap
Benefits of Backflushing
– More samples/day/instrument
– Better quality data
– Lower operating costs
– Less frequent and faster GC & MSD maintenance
– Longer column life
– Less chemical background
Three Other Devices Provide Backflush
Capability
2-Way Splitter with
Makeup
3-Way Splitter with
Makeup
Deans Switch
Pesticides: Three Way Splitter with Makeup
1X method with 1:1:0.1 split FPD:MSD:ECD
3-Way
Splitter with
Makeup Auto-sampler
7890
GC
Column
Phosphorus FPD
30 m X 0.25 mm id X 0.25 um HP-5MS
5975C
MSD
uECD AUX EPC
3.8 psig
Full scan TIC
SIM
µECD
5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00
FPD(P)
Milk Extract (1 injection)
5 10 15 20 25 30 35 40 45 50 55 60 65 70
Run stopped at 42 min and
backflushed at 280oC for 7 mins.
It took additional 33 mins
and column to 320oC to
remove these high boilers.
Blank run after backflushing
min
showing the column was clean.
Milk Extract
Dean Switch
Cut
Deans
Switch
Auto- sampler
7890A GC
FID1 FID2
Column 1 Column 2
Heartcutting 2-D GC provides extremely high
chromatographic resolution
Heart Cut to Column 2
Trace Sulfur Compound
(4,6-DMDBT)
Column 1 - FID 1
Column 2 – FID 2
0 2 4 6 8 10 12 14 16 18 min.
Hydrocarbon
Matrix
Diesel Fuel
2-D Separation of Sulfur Compound in
Diesel Fuel Compound is completely resolved and can be analyzed
with FID
Capillary Flow Technology solves difficult
application problems easily.
It opens up many new (and old)
possibilities for GC and GC/MS systems.
Summary
GC x GC background information
Why is the Application Important ?
Real-world samples can be too complex for sufficient separation on one chromatographic phase
Target analysis is very complex samples
Excellent visualization of the sample
Powerful technique for hydrocarbon class determination
Issues with current solutions
Non-integrated hardware
Lack of good data reduction software
Many based on thermal modulation requiring large quantities of cryo
7890A basic configuration
The configuration is simple to get started in flow modulated GCxGC
Split/splitless inlet, hydrogen carrier gas
PCM module
Modified TCD board
Three way modulation valve
Capillary Flow Technology modulator device
Two columns: 30m x 0.25mm non-polar, 5m x 0.25mm polar
FID at 200 Hz
7683 Auto Injector
Data processing
CG Image, LLC, Lincoln NE 68505
Zoex Corporation, Pasadena, TX 77505
Conventional GC has its limitations
Separation may be insufficient for complex samples
Petrochemical
Flavors and Fragrances
PCB’s
Coffee
Complex matrices: biological, soils
Comprehensive 2-D GC (GCxGC) basics
Consists of four parts:
1. A primary column (conventional separation)
2. A modulator
3. A second column (very fast separation)
4. Fast detector
The modulator does two jobs:
1. It collects effluent from the primary column
2. It transfers the collected effluent (in whole) to the secondary column This process is repeated approximately every 1.5 seconds, synchronized with the start of data acquisition GC x GC Chromatogram
The peak capacity of the system is the
product of the peak capacities of the two
columns: result – a lot of separation power
Peak capacity
GC x GC peak capacity is:
1000 x 25 = 25000 in this
example
ALS
Column 1
Modulator
Column 2
Detector
n= 1000
n = 25
Conventional GC
Fast GC
Basic system layout
7683
Auto-sampler
7890A GC
FID
Column 1 Column 2
Flow modulator
s/s inlet
PCM
Switching valve
modulated
2nd column
1st column
7683
Auto-sampler
7890A GC
FID
Column 1 Column 2
Flow modulator
s/s inlet
PCM
Switching valve
modulated
2nd column
1st column
7683
Auto - sampler
7890A GC
FID
Column 1 Column 2
Flow modulator
s/s inlet
PCM
Switching valve
modulated
2 nd column
1 st column
7683
Auto - sampler
7890A GC
FID
Column 1 Column 2 Column 2
s/s inlet
PCM
Switching valve
modulated
2 nd column
1 st column
Agilent’s flow modulator : Differential Flow
Using Design by John V. Seeley, Oakland University
Modulation
Valve
FID
Split/Splitless
Inlet
Column 1 (25 – 30 M)
Column 2 (5M)
Collection
channel
Flow Modulator
H2
Flush Flow
direction
Collect Flow
direction
Flow modulator eliminates the need for cryo. Sample compression controlled
by flow ratios occurs in the collection loop and is quickly injected into the second
column, resulting in very narrow and tall peaks.
Capillary Flow Technology- Design
• Photolithographic chemical milling for low dead volume
• Diffusion bond two halves to form a single flow plate
• Small, thin profile provides fast thermal response
• Projection welded connections for leak tight fittings
• Deactivation of all internal surfaces for inertness
… a proprietary Agilent Technology
Flow modulation device
Load or collect step
Modulation
Valve
FID
Split/Splitless
Inlet
Column 1 (25 – 30 M)
Column 2 (5M)
Collection
channel
Flow Modulator
H2
Collect Flow
direction
1 ml/min
20 ml/min
Load time must not be
longer than time to fill
collection channel
Inject step
Modulation
Valve
FID
Split/Splitless
Inlet
Column 1 (25 – 30 M)
Column 2 (5M)
Collection
channel
Flow Modulator
H2
Inject Flow
direction
1 ml/min
20 ml/min
Collection channel is
quickly “injected” into
second column in about
0.1 seconds
20 ml/min
Chromatographic parameters
Agilent 7890A
Inlet: Split/splitless
Detector: FID
Data rate: 200 hz
Other pneumatics: PCM
Auto injector: 7683
Syringe: 5 ul
Carrier: Hydrogen
Inlet Pressure: 21.5 at 50 oC, constant flow
PCM: 20 ml/min, constant flow
Oven Program: 50 oC (1.0min) to 260 oC (4 min) @ 5 or 8 oC/min.
Typical modulation parameters
Modulation start: Synchronized with
start of data
acquisition
Modulation Valve on: 0.12 seconds typical
(Inject)
Modulation Valve off: 1.40 seconds typical (load)
Collection channel: 15 cm x 0.45 mm ID
Three-way valve: HP19232-60570, 12VDC
N-butylbenzene
11.8 11.85 11.9 11.95 11.75 11.8 11.85 11.9 11.95
unmodulated modulated
Kerosene raw data Alkane, mono-aromatic, and di-aromatic
separated in 1.5 seconds
Zoom from 15.8 to 16 min
Heavy gasoline raw 2D data
Note hydrocarbons being separated
in each 1.5 second modulation
GC X GC modulation basics
1.Acquisition
2. Transformation
1D-GC chromatogram (at the end of the 1st column in blue)
9 modulations shown
Coelution of 3 compounds!
Raw 2D-GC
chromatograms
(at the end of the 2nd column)
Take “slices” of the co-eluting
peaks and inject quickly to
another column of different
selectivity
“red” peak elutes last now and “green” peak elutes first and all 3 completely separated!
1
2
3
4 5 6
7
8 9
GC X GC visualization
2nd Dimension
chromatograms stacked
Reconstitute the peaks by
combining each of them from
each chromatogram
2D Image
1st Dimension
2nd D
ime
nsio
n (
fast G
C)
Chromatograms produced
by 8 modulation cycles
System performance check mixture: 7890A
1
2 1
3
4 5
6
7
8
9
10 11
12
13
14
15
16
17
18 1
2 1
3
4 5
6
7
8
9
10 11
12
13
14
15
16
17
18
1. Octane
2. Fluorobenzene
3. Propylbenzene
4. Bromo-2-fluorobenzene
5. Indane
6. Butylbenzene
7. Tetralin
8. Dodecane
9. Naphthalene
10. Tridecane
11. Tetradecane
12. Fluorobiphenyl
13. 1,3,5-Tributylbenzene
14. Acenaphthalene
15. Fluorene
16. Terphenyl
17. 2-Methyl anthracene
18. Eicosan
Mixture of wide boiling point and polarity
Flow modulation: Straight run heavy gasoline
7890A
naphthalenemethyl-naphthalenes
naphthalenemethyl-naphthalenes
Column 1: HP-5MS 30m x 0.25mm x 0.25um
Column 2: INNOWAX 5m x 0.25mm x 0.15um
Flow modulation:
(GC x GC) of diesel fuel: 7890A
GC x GC Image:
• Showing the normal B.P. distribution (1st dimension)
• Also shows the hydrocarbon class clusters
• Consistent RT for alkanes in 1st dimension showing precise modulation
• Comparable peak in 2nd dimension band shows minimum peak broadening
with flow modulation
Naphthalene
Toluene
p-xylene
o-xylene
C9 C12 C16
Alkanes
mono-Aromatics
di-Aromatics
Methyl-naphthalenes
Flow modulation:
(GC x GC) of Kerosene: 7890A
Modulation
1.40 second collect
0.11 second inject
Column 1: HP-5MS 30m x 0.25mm x 0.25um
Column 2: INNOWAX 5m x 0.25mm x 0.15um
Oven rate: 8 oC/min
Mono-aromatics
Di-aromatics
Alkanes
Kerosene at 5 oC/min: 7890A
alkanes
cyclic alkanes
mono-aromatics
di-aromatics
alkanes
cyclic alkanes
mono-aromatics
di-aromatics
Slowing the oven program rate to 5 oC/min improves group separation
Column 1: HP-5MS 30m x 0.25mm x 0.25um
Column 2: INNOWAX 5m x 0.25mm x 0.15um
Modulation
1.40 second collect
0.11 second inject
Flow modulation:
(GC x GC) of B20 biodiesel fuel: 7890A
Modulation
1.40 second collect
0.11 second inject
alkanes
C16:0
C18:2
C18:1
C18:3
C18:0
mono-aromatics
di-aromatics
FAMES
Separation of 4,6-Dimethyldibenzothiophene in
diesel
4,6-Dimethydibenzothiophene
Separate run with
just the dibenzothiophenes
4-Ethyl,6-methyldibenzothiophene
Flow modulation: Detergent perfume base:7890A
2D GC is ideal for application of
pattern recognition techniques
to determine product quality,
authenticity, adulteration, etc.
Small degree of wrap around on this compound
Summary for Agilent flow modulation GC x GC
• Reliable Setup: Based on capillary-flow- technology, easy to setup, high performance
chromatography, and reliable.
• High temperature operation: Operation to 350 C expands applications
• No Cryogen Required: Flow modulation means no tanks of Liquid N2 or CO2
• 7890A Enabled GC x GC: Capillary- flow-technology ready, synchronized periodic events
ensure precise modulation, control from modified TCD board
• Comparable resolution without N2: Cap Flow Technology allows low dead volume and
precise flow control, resulting in minimum peak broadening even without cryo-focusing . Peak
widths on the second column are typically 60 to 100 ms at half maximum.
• Sensitivity: Approaches that obtained by thermally modulated systems
Agilent LTM (Low Thermal Mass)
Rapid Heating/Cooling System for GC, GC/MS
“LTM” (Low Thermal Mass) Technology
Direct heating of fused silica GC columns
LTM Cooldown Times (Standard Size)
0
50
100
150
200
250
300
350
400
0 50 100 150 200 250
Time (sec)
Tem
p (
oC
) 2m LTM
5m LTM
10m LTM
7890 GC
Additional Cooldown times available on website
for LTM column modules up to 30m
Interfacing LTM GC to an Agilent Gas Chromatograph
Modules outside isothermal GC oven for fast heating/cooling
Use same GC injectors, detectors, autosamplers, software, …
Independent and simultaneous
temperature programming of:
1-2 col modules (standard, fast cool) 90% sales
1-4 col modules (small)
Note: Front thermal shield removed to show LTM column modules
Entire thermal shield should always be in place during operation
LTM Column Modules
(standard width shown)
LTM Control System
w/ Keypad User Interface
… Agilent Control SW now available to order
Agilent LTM Control Software
(Examples of Preliminary Screens)
pA
0
1000
2000
3000
4000
5000
6000
min 0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.25
C5
C6
C7
C8
C 9
C10
C11
C12
C14
C15
C16
C17
C18
C20
C24
C28
C32
C36
C40
pA
min 0.25 0.5 0.75 1 1.25 1.5 1.75 2 0
500
1000
1500
2000
Fast Simulated Distillation Under 3 Minutes Using LTM
… 6x faster compared to conventional ASTM D2887 procedure
ASTM D2887 Reference Oil
LTM Module : 45ºC to 350ºC at 150ºC/min
Faster than conventional GC (75-120oC/min max)
Calibration sample C5-C44
LTM Module : 45ºC to 350ºC at 150ºC/min
min0 0.5 1 1.5 2 2.5
pA
0
100
200
300
400
500
600
700
800
900
General retention time repeatability data [by Agilent/Roger Firor]
at LTM website – “Technology” section or “FAQ”
Retention time repeatability – similar to conventional GC
Overlay of 10 runs
Cracked gas oil: 45ºC to 350ºC at 150oC/min
Environmental/Food Safety/Forensics
Need for high through-put, especially for low margin samples, where analytical cycle times are a critical element in cost per analysis
Key Sales Tools 5990-3201EN Ultra-Fast Total Petroleum Hydrocarbons (TPH) Analysis with Agilent Low Thermal Mass (LTM) GC and Simultaneous Dual- Tower Injection (Wei & Szelewski) - 9x faster TPH throughput using LTM - 18x faster TPH using LTM and dual simultaneous injection
5990-3451EN Fast Analysis of Polynuclear Aromatic Hydrocarbons Using Agilent Low Thermal Mass (LTM) GC/MS and Capillary Flow
Technology Purged Union for Backflush
- 2x faster PAH runs using LTM, even faster with Backflush - Enviro and Food Safety samples can be dirty. LTM columns cannot be trimmed (not Agilent, not Thermo…) - LTM uses guard columns…and now Backflush/CFT Backflush delivers multiple benefits for LTM analyses incl reduced. potential for carryover, longer column life, shorter analysis time
6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 Time-->
3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 Time-->
Reference method – Standard Oven
30 m x 0.25 mm ID x 0.25 µm DB-5MS
Fast Analysis - LTM
20 m x 0.18 mm ID x 0.18 µm DB-5MS
PAH by
LTM/GC/MS
Column contamination
from just one prior run
5.00 5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80
Time (min)
Contamination free when
using backflush
PAH by
LTM/GC/MS
Productivity Benefits of Backflush
(Backflush Flyer = 5989-9804EN)
• More samples per day per instrument
• Longer column life
• Lower operating costs
• Less frequent and faster GC & MSD maintenance
• Less chemical background
– More consistent retention times
– More consistent baselines
– Higher quality spectra (no increase in noise during analysis
sequence)
– Higher quality quantitation (no increase in interfering ions
during analysis sequence)
References for Backflush
5989-9359EN Capillary Flow Technology for GC/MS: Efficacy of the Simple Tee Configuration for Robust Analysis Using Rapid Backflushing for Matrix Elimination (Prest, Foucault, and Aubut, Aug 08)
5989-9341EN Screening for 430 Pesticide Residues in Traditional Chinese Medicine Using GC/MS: From Sample Preparation to Report Generation in One Hour (Luan, Xu, Sept08)
5989-8664EN Capillary Flow Technology for GC/MS: a Simple Tee Configuration for Analysis at trace Concentrations with Rapid Backflushing for Matrix Elimination (June 08, Prest)
5989-8588EN The Use of Automated Backflush on the 7890A/5975C GC-MS System
5989-8582EN Improved Forensic Toxicology Screening Using A GC/MS/NPD System with a 725-Compound DRS Database (Quimby, May08)
5989-7670EN, Replacing Multiple 50-Minute FPD/ELCD/SIM Analyses with One 15-Minute Full-Scan Analysis for 10x Productivity Gain (Meng/Szelewski, Nov07)
References for Backflush
5989-6460EN Analysis of Suspected Flavor and Fragrance Allergens in Cosmetics Using the 7890A GC and Capillary Column Backflush (March 2007)
5989-6095EN Direct Injection of Fish Oil for the GC-ECD Analysis of PCBs: Results Using a Dean Switch with Backflushing (Jan 2007)
5989-6066EN Rapid Forensic Toxicology Screening Using an Agilent 7890A/NPD/5975C/DRS GC/MSD System (Jan 2007)
5989-6018EN Improving Productivity and Extending Column Life with Backflush (Dec 2006)
5989-5111EN Simplified Backflush Using Agilent 6890 GC Post Run Command (June 2006)
5989-1716EN New Tools for Rapid Pesticide Analysis in High Matrix Samples (October 2004)
LTM Also Greatly Reduces Cool-Down Times,
9x Faster Heating/Cooling Cycle Times
40 min + 5.4 min
20 min + 5.4 min
3 min + 2 min
GC Run Time Cool Down
LTM/7890
9x Faster
Cycle Time (200oC/min)
Food/Flavor/Fragrance and Pharmaceutical
Chiral Separations
• Chiral GC is most effective at low temperatures, yet complex samples usually require a broad temperature program to separate target compounds from background and to elute highly retained sample components.
• LTM/GC/MS uses a traditional column in the GC oven to separate target compounds, then heart-cut of target compounds to a chiral column in LTM module at a lower temp. optimal chiral separations are achieved while decreasing analysis cycle times and
increasing chiral column lifetime. 5990-3428EN Independent Temperature Control Using an LTM Oven Module for Improved Multi-dimensional Separation of Chiral Columns - 2D LTM/GC/MS, simultaneous/independent temperature programming of GC and LTM column module(s) Article Multidimensional Gas Chromatography with Capillary Flow Technology and LTM-GC, J Luong (et. al) Dow Chemical,R Mustacich Published:Journal of Separation Science, ISSN 0021-9665, Volume 31, pp. 3385-3394253-261 - Examples 2D LTM/CFT/GC using Deans Switch and LTM’s simultaneous/independent temperature programming
Heart-cut
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Conventional GC/MS–Both columns in Single Oven, Single Deans Switch
Low Level (0.5 ng/ml) THC in Blood Difficult to Detect, Many Interferences
LTM/GC/MSD–Independent Column Thermal Profiles, Dual Deans Switch
Low Level Detection (0.5 ng/ml) THC in Blood, Good Resolution
Run Time Reduced from 15 minutes to less than 11 minutes
LTM Products
Column Modules
% Size #/System Feature
> 90% Standard (5”) 1-2 Fastest Cooling
< 10% Small (3”) 1-4 Up to 3-4 Mod’ls
Capillary Column - up to 30m maximum
LTM System
For Agilent GC: 7890 or 6890 (not 5890)
(New 7890 requires #650 “LTM
Ready”
Different P/N’s for: 7890 vs 6890 (Door Mountings)
New 7890 vs Existing 7890/6890
Standard vs Small Format
# Channels (= # Col Modules)
G6579A (2 channel, standard)
plus 2 Column Modules
G6578A (1 channel) + 1 Col Module
LTM Software G6586AA
Gracias por vuestra atencion
