Význam tématu
Optimalizace spojení kapilárních GC/GC-MS systémů je klíčová pro spolehlivost analýz, minimalizaci úniků a zachování inertnosti toku vzorku. Správné spojení prodlužuje životnost kolony, snižuje dobu údržby a zlepšuje reprodukovatelnost výsledků.
Cíle a přehled studie
Cílem textu je představit inovativní nástroje a spotřební materiál od společnosti Agilent, které usnadňují montáž, zaručují trvalou těsnost a inertnost spojů a zvyšují produktivitu v rutinní chromatografii.
Použitá metodika a instrumentace
Pro zajištění konzistentních spojení byly analyzovány následující komponenty a postupy:
- Typy ferrulí: polyimidové, grafitové, polyimid/grafit (85/15 %), flexibilní kovové UltiMetal Plus.
- Maticové spoje: standardní, finger-tight“ Self-Tightening Column Nuts s pružinovou patronou.
- Přístrojové vybavení: Agilent Intuvo 9000 GC/GC-MS, Intuvo Flow Chips, Guard Chips, Ultra Inert Press Fit konektory, UltiMetal Plus tubing a fittings.
- Srovnávací testy těsnosti a inertnosti při teplotních programech a opakovaných cyklech (až 400 běhů).
Hlavní výsledky a diskuse
- Self-Tightening Column Nuts udržely optimální těsnost bez nutnosti opakovaného dotahování i po 400 cyklech, čímž eliminovaly základnu šumu způsobeného úniky.
- UltiMetal Plus ferrule s povrchovou úpravou významně snížily aktivity na povrchu a zlepšily detekovatelnost stopových organofosfátů.
- Ultra Inert Press Fit konektory i Intuvo Flow Chips zajistily rychlé, opakovatelné spojení bez mechanického poškození kolony.
- Planární kolony Intuvo bez nutnosti stříhání zjednodušily údržbu a eliminovaly chyby při měření instalační délky.
Přínosy a praktické využití metody
- Snížení prostojů laboratoře díky beznástrojovým spojům a okamžitému kliknutí při správné instalaci.
- Zlepšení přesnosti a citlivosti analýz díky trvale inertním spojům a eliminaci aktivit na stěnách spojů.
- Univerzální použití v GC, GC-MS, Capillary Flow Technology, včetně aplikací backflush a multidimenzionální GC×GC.
Budoucí trendy a možnosti využití
- Další rozvoj materiálů ferrulí s vyšší tepelnou stabilitou a nulovou permeabilitou vzduchu.
- Integrace inteligentních čipů do dalších částí GC toku pro automatické sledování životnosti spotřebního materiálu.
- Rozšíření „click-and-run“ spojů do plně automatizovaných laboratorních linek a vzdálené diagnostiky úniků v reálném čase.
Závěr
Představené inovace od Agilent představují výrazný krok k spolehlivější a efektivnější chromatografii. Kombinace self-tightening matic, UltiMetal Plus ferrulí, press-fit konektorů a Intuvo Flow Chips umožňuje laboratorním specialistům dosahovat konzistentních výsledků s minimální údržbou.
Použitá instrumentace
- GC/GC-MS systémy Agilent Intuvo 9000
- Self-Tightening Column Nuts (P/N 5190-5233, 5190-6194)
- UltiMetal Plus flexibilní kovové ferrule
- Ultra Inert Press Fit konektory
- Agilent Intuvo Flow Chips a Guard Chips
Obsah byl automaticky vytvořen z originálního PDF dokumentu pomocí AI a může obsahovat nepřesnosti.
Optimizing your your Current
GC/GCMS with Better Connections
Introducing The Agilent
Intuvo 9000 Easy leak free GC Click
& Run Connections
Abby Folk
Columns and Supplies Online Applications
GC column installation is a challenge…
A routine, basic procedure but not easy to do
• Very small parts
• Wrenches in cramped, dark space
Two chances to get it wrong:
at the inlet and the detector
What can go wrong?
• Height into the fitting
• Leaks
• Activity
2
How do you make better GC column connections?
1. Start with the right tools and supplies
• Column nuts
• Material : stainless – but need brass for MS interface
• Choice of right ferrules
2. Proper assembly process
• Make a good clean column cut – every time
• After ferrule is installed
• Fused silica tubing cutters : ceramic, diamond tipped etc.
• Magnifier to inspect the cut - cracked fused silica and flaps of polyimide
are active sites that ruin chromatography.
3. Ensure the proper and consistent length of column into the fitting
3
polyimide
Supply Selection: Which Capillary Ferrules to use?
Composition
Re-use
Max T
Use
Limitation
Polyimide (Vespel)
yes
280
Easy seal
Shrink after heating causing leaks after
thermal cycle; isothermal only
Graphite
yes
450
FID, NPD Inlets
Contamination, permeable to air
– not
for oxygen sensitive detectors
Polyimide/graphite
(85% / 15%)
limited
350
MS, ECD, Inlets
Still shrink after thermal cycles creating
leaks; need to retighten regularly
Flexible metal
no
450
Capillary Flow
Technology
(backflush,
splitters,…)
May not seal well with damaged fittings
or rough surfaces
4
polyimide/graphite
graphite
“Long” ferrules for MS transfer lines and MS interface nut
“Short” ferrules for inlet and detector configurations on Agilent GC’s
flexible metal
Supply selection: Graphite Ferrules
Often selected because
• high temperature range (450C)
• the least expensive capillary ferrules
• Soft, easily conform to fitting shape and size
But do not over tighten!
Over tightening of ferrules
• Causes ferrule material to extrude into the fitting
• Creates active sites if in the flow path
• Can flake or fall apart, blocking flow path and requiring
extensive maintenance
Remember Graphite is NOT recommended with MS,
ECDs or with any Capillary Flow Devices. Graphite is
permeable to air be very careful.
Active sites in the flow path
Extensive Inlet maintenance
needed
5
Supply Selection: Graphite/polyimide blend ferrules
Graphite / polyimide (vespel) blend ferrules are very popular
• Recommend
• Long style for Mass Spec
• Short for Inlets, and other oxygen sensitive detectors, like ECD
• Soft enough to make seal against rough surfaces
• Fairly high temperature stability (350C)
• Don’t extrude beyond the fitting when tightened (like graphite)
• Lower air permeability than pure graphite
6
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
7
Capillary column nuts
Column nuts are determined by the
instrument fitting
Basic mechanical fittings with little
enhancements
• Brass for the MS
• Some finger tight designs for ease
of use
New design addresses ease of use
and productivity issues of leaking
and over tightening
8
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
9
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!
10
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!
11
How do you make better GC column connections?
1. Start with the right tools and supplies
• Choice of right ferrules = short graphite/polyimide
• Column nuts = Self Tightening
2. Proper assembly process
• Make a good clean column cut – every time
• After the ferrule is installed
• Fused silica tubing cutters: ceramic
• Magnifier to inspect the cut - cracked fused silica and flaps of polyimide
are active sites that ruin chromatography
3. Ensure the proper and consistent length of column into the fitting
12
Column installation assembly process
1. Thread through an
inlet septum
2. Pass column through
the column nut
3. Install ferrule onto the
column tubing
4. THEN make a fresh
cut
5. Inspect the cut; repeat
cut if any jagged or
rough edges
1
2
3
4
5
13
Installation Distance Matters
Ensure the proper length …
Column Installation Tools
Follow the manufacturer’s recommended procedure
• Optimized GC performance and reproducibility requires
ensuring the proper length of column into the fittings, every
time
• Column Installation pre-swaging tools for the
Split/Splitless, Multi Mode and Purge Packed Inlets
available for Agilent GC models 7890/7820 and 6890/6850,
for graphite or metal ferrules
G1099-20030
MS Install Tool
G3440-80217 Graphite Ferrules Metal Ferrules G3440-80218
15
Pre-swaging Tool for CFT Devices
.
Advanced techniques increase the number of
connections
Simple addition of a retention
gap or guard column doubles
the column connections
Powerful advanced GCxGC
systems with many
connections
17
Better connections: Beyond the basics
Sample splitting for productivity:
•
Split effluent from a single column to 2
or more detectors on the same GC.
•
Backflush
– replacing a “bakeout” for
high-boiling analytes that collect in the
column then interfere with subsequent
analyses
GC x GC or 2-dimensional GC
•
An approach used in some
environmental, food and flavor, and
hydrocarbon processing applications
•
Separates complex mixtures using two
independent columns with different
stationary phase selectivity
•
Columns are connected in series and
separated by a modulator
Limitations to Adoption of :
All column connections must:
•
be inert, not adsorbing or decomposing
analytes
•
have low thermal mass and low dead
volume to maintain sharp peak shapes
•
be leak free
– and stay so
•
not outgas from materials used to
make the seal
•
withstanding the temperatures used in
the GC analysis
•
not be technique dependent
– must be
easy to do
18
Blood Alcohol Analysis: The Problem with Splitters
Two holed ferrules are inexpensive and straightforward to
use. Their challenges are:
1. Poor inlet dynamics
2. Unpredictable splitting
3. Requires a larger holed gold seal
4. Crowding in single taper inlet liners
5. Lack of guard column when used in the inlet
These devices resolve some of the issues but are not
very popular.
19
Blood Alcohol Analysis: The Problem with Splitters 2
•Why can’t I get my Press-Union connector to seal?
Press-Union connectors are easy to use, but if they are not properly sealed,
they can loosen due to thermal expansion during temperature-programmed
runs. The keys to successful sealing are: 1) making a clean, square cut on the
column and 2) moistening the end of the column with methanol or acetonitrile
before seating it into the connector. A small amount of polyimide resin also
helps prevent the seal from separating during temperature cycling.
The glass “Y” splitter overcomes many of the challenges of the 2
holed ferrule and adds expense.
However installing the connector is somewhat of an art, and even
then it is prone to leaking. Unpredictably.
20
Better Connections: Glass column connectors
Ultra Inert Press Fits
Join retention gap or guard column to analytical, or split effluent
Dependable inertness performance at a lower cost
Improved robustness, holding strength
Batch certified inertness
Improved packaging and installation instructions
Easier to use - transparent deactivation gives visibility of the
column connection
Ultra Inert Press Fit
Traditional Deactivated Connector
21
Blood Alcohol Application: Agilent Solution
7890B
GC
S/S
Inlet
FID
CH
2
FID
CH
1
Un-Purged
Splitter
0.4 m x 0.45
mm Retention
Gap
Column 1: DB-
ALC1
Column 2: DB-ALC2
7697A
Headspace
Sampler
HSS
Transfer
Line
G3445B#683
22
Better Connections: Capillary Flow Technology Devices
UltiMetal Plus Ultimate Union/UltiMetal Plus Tee
• Stainless Steel Micro Fluidic plates technology
• Deactivation essential to block active sites
• Column connection easy to assemble Release hole for
stuck ferrules
Using Flexible Metal ferrules to overcome issues
• UltiMetal Plus surface chemistry prevents activity
• Flexible design reduces risk of over tightening or column
breaks
• Leak free seal remains after repeated temperature cycles
23
Vespel
Ferrules
Composition
Re-use
Max T
Use
Limitation
Vespel
yes
280
Easy seal
Leaks after T cycle, iso only
Vespel/graphite
limited
350
MS
Retighten after T cycle
Graphite
yes
450
Not MS
Contamination, leakages
Siltite
yes
450
MS, CFT
Column breakage
24
Vespel/graphite
Dial packaging
Graphite
Siltite
“Long” ferrules for MS transfer lines and MS interface nut
“Short” ferrules for detector and inlet configurations
on Agilent GC’s, provide a robust seal.
Flexi-Metal Ferrules: Touchless Dial Packaging
Clear installation instructions
o Easy column insertion
o No lost ferrules
o No contamination risks
25
Flexible Metal Ferrule Design Features
Grooves
reduce bulk stiffness during
compression and improves ID
constriction.
Angle eliminates wall frictional
contact to allow the material to
flow into the ID area for larger
range of constriction.
Tighter ferrule ID
specification and
tolerances (30%)
Wider opening
allows for easier
column insertion
1
2
3
4
26
Current Ferrule
Stiff, prone to cause
damage to column
or fitting
Small ID compression
(40 to 60um)
– leaks
Tolerances poorly
controlled
Quality issues
▪ mixed inventory
▪ not-fitting
▪ column crushing
▪ leaking
Agilent
Flexi-Metal Ferrule
Computer aided Design
Finite Element Analysis
More flexible
Less column damage
Large range of
ID compression
(100 to 120um)
– less leaks
Agilent design alleviates current
quality issues
Compare current to new Agilent ferrule
More Added Value
Agilent Intellectual Property:
Utility patent & Design patent
applications
Exclusive Agilent product
New UltiMetal Plus surface treatment
provides excellent ferrule inertness
exceeding Siltite performance
Page 28
Each ID has its own unique design
Ease of recognition, no mix-ups
Family of ferrules for range columns
Folsom and Middelburg including
Ultimetal columns, and a no hole plug
Impact of ferrule surface on inertness
29
4
x10
0
1
2
4
x10
0
1
2
Counts vs. Acquisition Time (min)
4.5
5
5.5
6
6.5
7
7.5
Untreated FMF
Post column Std 500ppb
FMF + UltiMetal Plus
Post column Std 500ppb
Acephate
Omethoate
Demeton-S
Acephate
Omethoate
Demeton-S
Very small amount of ferrule surface exposed to active pesticides
Flexible Metal Ferrules
Positioning
Substitute for Siltite ferrules in
All CFT devices
QuickSwap
Backflush
Ultimate union
LTM
Not optimized for regular Agilent inlet / detector connections
but possible! Graphite/vespel ferrules allow more
economical column trimming and re-tightning
“Long” ferrule
applications
30
“Short”
ferrules
Summary
Agilent Flexible Metal Ferrule
Family of novel, patented design capillary column metal ferrules
Capillary Flow Technology fittings
Agilent GC inlets and detectors
MS interface.
▪ Reduces risk of over tightening and breaking column
▪ Leak free seal after repeated temperature cycles
▪ UltiMetal Plus chemistry prevents loss of active analytes
Ease of Use
▪
Easy assembly and tighten to give a leak free seal (“forgiving”)
▪ Ferrule ID identification by design
▪ Quick installation due to design & packaging
31
Agilent UI Gold Seal: Deactivated gold surface
•Soft gold plating is essential for proper sealing
•Ultra Inert chemistry blocks active sites (gold is NOT
inert)
•Smooth surface doesn't leak
•Advantage Agilent
•P/N 5190-6144 ea, 5190-6145 10 pack
32
Agilent MIM seal
Competitor’s
machined seal
Reliable ppb and ppt
measurements require
attention to the little things!
Better connections: UltiMetal Plus Tubing and Fittings
• UltiMetal Plus Deactivated metal
tubing and valves
• 0.53 and 0.25 mm ID guards and
transfer lines
• Metal fittings (unions, tee’s and nuts)
• Steel tubing (1/16”, 1/8”, ¼”)
• Ultimetal Plus fused silica guard
columns
Ensure the entire chromatographic solution is inert and corrosion resistant
to provide superior performance with improved peak shapes
even for active compounds
33
Making Better GC Connections
• Select supplies appropriate for your instrument and
application
• Follow recommended assembly process
• Maximize productivity by using innovative tools and supplies
➢ Column Installation Pre-swaging Tools
➢ Self Tightening Column Nuts
➢ Ultra Inert Press Fit Connectors
➢ UltiMetal Plus Flexible Metal Ferrules
➢ UltiMetal Plus Tubing and Fittings
34
Agilent Inert Flow Solution
Ultimetal Plus
– TCD, FPD, NPD/FID Jets
Inert MS Source
Ultimetal Capillary Flow Technology
Devices, Ultimate Union
Ultra Inert GC Column
Ultra Inert Gold Seal
Ultra Inert Inlet Liner
Ultimetal Plus Ferrules
Ultimetal Plus Inlet Weldment, Shell
and Transfer Lines
35
21.00
21.50
22.00
22.50
23.00
23.50
24.00
400
1200
2400
1. Temazepam
2. Flunitrazepam
3. Diacetyl
morphine
4. Nitrazepam
5. Clonazepam
6. Alprazolam
1
2
3
4
5
6
Green = Inert Flow Path
Blue = Standard Flow Path
Drugs of Abuse 0.25 ng Column SIM Mode
Putting It All Together — Agilent Inert Flowpath
Dramatic Improvement at Low Levels
36
The New Agilent Intuvo 9000 GC System
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
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
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
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
No More
- measuring
- over-tightening
- trimming
A New Portfolio of GC Consumables
UI Inlet Liners
Guard Chip
No-trim
column
Intuvo
Flow
Chips
Smart Keys
Tools &
Accessories
Intuvo Flow Chips – Installation distance perfect always
No More
- Measuring
- Over-tightening
- Trimming
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.
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!!
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
Intuvo Flow Chips – UI Fixed Length Flow Paths
Where Does it Get Dirty?
Here
Here
Here
Here
Here
Here
Page 50
Not the Column!
New Autonomous Leak Checking
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
Now it’s easier than ever to get reliable GC results
through better GC connections from Agilent
www.agilent.com/chem/betterGCconnections
54
Order the poster…
View the video…
Questions
55
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
