CryoTrap - JAS - Joint Analytical Systems GmbHSplit˜ratio:˜1:50 GC oven:˜40→...
Transcript of CryoTrap - JAS - Joint Analytical Systems GmbHSplit˜ratio:˜1:50 GC oven:˜40→...
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CryoTrapFor Agilent Technologies 7890/6890/6850 GC Systems
CryoTrap
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Bad peak shapes and interferences of low boiling compounds are often observed in case of using a sample introduction other than liquid injection, such as headspace, thermal desorption or sampling loop for gas analysis.
In order to improve peak shape and peak resolution in the chromatogram it is required to refocus high
volatile components in the front of the column before chromatographic separation. Otherwise incorrect peak
identification and peak integration may occur.
The JAS double chamber CryoTrap is a powerful tool of high quality to efficiently trap volatile compounds in
the front part of a capillary column. It combines the latest advances in CryoTrap technology including low
thermal mass, efficient insulation and maximum heating power - features that ensure a fast heating and an
economical cooling. Various appropriate coolants can be used to cool the trap (liquid carbon dioxide, liquid
nitrogen and pressurized air). An extremely fast but controlled heating of the trapping zone up to 700°C/ min
allows a rapid re-vaporization of the trapped components for subsequently GC analysis – replacing a
high speed injection. As a result low boiling compounds occur as sharp peaks with a high resolution in
the chromatogram. JAS CryoTrap can be actuated either due to control software embedded into Agilent
ChemStation or by GC keyboard.
JAS CryoTrap is provided to be fully integrated in
Agilent 6890 and 7890 GCs. It can be positioned
inside the GC oven, either at the left hand side wall of
the GC oven or below the valve cabinet. The devise
requires one heated zone (150W) and one pneumatic
inlet slot of the GC. In case of Multi Dimensional GC
applications, JAS CryoTrap can also be mounted
outside the GC oven and connected to a second GC
by means of an optional heated transfer line.
Features
Features
The main advantageous features of JAS CryoTrap system are:
Flexible In order to meet your analytical needs JAS CryoTrap can be installed at various positions (two locations inside the GC oven and one location outside). Additionally, three different cooling options (liquid CO2, liquid N2 and pressurized air) provide complete flexibility to guarantee the most effective analytical conditions.
Efficient By means of a double chamber design the JAS CryoTrap features an effective insulation reducing the coolant consumption to a minimum.
Easy to Use Dedicated and optimized alignment of tuning parameters provides excellent performance at any oven temperature
Economical JAS CryoTrap is controlled either by Agilent ChemStation software or by GC keyboard. The use of the Trap is easy and may be embedded into every GC method.
Fig. 1
JAS CryoTrap
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Column in Column in
Column out
OUT
Liquid coolant
IN
Gaseous coolant
Column out
HeatingCatridge
Cooling Phase Heating Phase
Operating Mode
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00
1000000
2000000
3000000
4000000
5000000
6000000
7000000
8000000
9000000
1e+07
1.1e+07
1.2e+07
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00
5000000
1e+07
1.5e+07
2e+07
2.5e+07
3e+07
3.5e+07
4e+07
4.5e+07
5e+07
2
Time (min)
Abu
ndan
ce
Abu
ndan
ce
Ace
ticac
id
Furfu
ral 3-
Met
hylh
ydan
toin
Without CryoTrap
GC-Method: 40°C for 6 min, with 20°C/min to 300°C
Time (min)
Ace
ticac
id Furfu
ral
3-M
ethy
lhyd
anto
in
CO
With CryoTrap
GC-Method: 40°C for 4 min, with 15°C/min to 300°C
The outer wall of the JAS CryoTrap is made of stainless steel. In order to resist thermal fluctuation a tube of a
specific material for optimal heat carriage is inserted into the CryoTrap body.
The analytical column is guided through the CryoTrap chamber. Due to appropriate coolants the trap is cooled
down to the effective temperature and components transferred from the inlet system to the analytical column
are trapped before chromatographic separation. Re-vaporization for subsequent GC analysis is caused by
means of rapid but controlled heating of the trapping zone. Temperature and time of trapping process can be
optimized depending on the analytes and may easily be adjusted using the control software. A fast heating
rate is important in order to obtain sharp peaks of volatile components. As a result peak broadering and
interferences are minimized and quantitative evaluation becomes more precise.
Chromatograms of a wood sample are illustrated for comparison. Figure 3a shows the bad quality of
peak resolution for high volatile components, like acidic acid or furfural, in case no Cryo Trap is used. An
identification and integration of these peaks with reasonable certainty is not possible. Figure 3b demonstrates
the necessity of using a CryoTrap in order to improve the peak resolution of low boiling compounds.
Fig. 2
Functionality of JAS CryoTrap
Fig. 3a
Analyses of high volatile compounds in wood samples
Fig. 3b
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2.5e+07
Benz
ene
1.5e+07
2e+07
TD-GC/MS: Thermal desorpt ion(200→320°C wi th CryoTrap)
5000000
1e+07
HC
l
Hydrochloric acid8000000 Ion 36.00 (35.70 to 36.70):
Carbon dioxidem/z=44
m/z=36
3000000
Ion 44.00 (43.70 to 44.70):
Acetic acidm/z=601500000
Ion 60.00 (59.70 to 60.70)
/1500000
Ion 100.00 (99.70 to 100.70)
m/z=100 2-propenoic acid (methyl ester)
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
TD-GC/MS: Thermal desorption(200→320°C without Cryo Trap)
1400000
Abundance
Column: UA5 (30m, x 0.25mm x 0.25μm)PyrolyzerFurnace: 200ºC→320ºC (20°C/min)Carrier gas: He 1ml/minSplit ratio: 1:50GC oven: 40→ 20ºC/min→320ºC (1min)Injector: 320ºC
1100000
1400000
These are residual volatiles which can be separated by cryo-trapping during desorption.
800000
500000
1 00 00 10 00
200000
1.00 5.00 10.00Time (min)
Operating Mode
Figure 4:
Comparison of thermal desorption analysis (200– 320°C)
with (4a) and without (4b) Cryo Trap (TD-GC/MS system)
4a
4b
Thermal desorption often results in broad initial
peaks including numerous individual components.
While reducing of the initial column temperature or
using thick film columns will just narrow this initial
band width, cryo-focussing is the most efficient and
cost effective way of ensuring peak separation.
Figure 4a and b illustrate the separation
improvement of the volatile fraction by means of
cryo-trapping. Qualitative and quantitative data
quality will be enhanced tremendously.
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Specifications
Specifications of JAS CryoTrap
Description Double chamber CryoTrap design with combined inlet/exhaust port
Order Numbers for GC 6890: for GC 7890:
JAS 65600 JAS 66600 - for air cooling JAS 66601 - for liquid N2 JAS 66602 - for liquid CO2
Instrument Dimensions Length: 105 mm Width: 20 mm (o.d.) / 1 mm (i.d.)
Compatibility Agilent GC 7890/6890/6850
Power Int. Power Supply 24V, Input 150 VA
Maximum Temperature Agilent GC 6890: 500°C Agilent GC 7890: 450°C
Cooling Temperature Liquid N2: -160°C Liquid CO2: -60°C
Pressurized Air: ambient temperature or oven start temperature
Heating Rate 1-700°C/min
In case of Multi Dimensional GC application the JAS CryoTrap is positioned outside the oven to trap
components eluting from the first separation column.
Using liquid nitrogen as cooling agent a dewar vessel with a dip tube is required (minimum 1 bar head
pressure for full perfomance mandatory). In case of liquid carbon dioxide as cooling agent a cylinder with
a dip tube and a variable restriction is required.
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Carl-Zeiss-Str. 49
47445 Moers
Germany
Phone: +49 2841 9871 100
Fax: +49 2841 9871 222
e-Mail: [email protected]
Internet: www.jas.de
joint analytical systems GmbH
About joint analytical systems
Since 1995 JAS is a major partner and Value Added Reseller of Agilent Technologies. We are an innovative-driven organization that offers customized solutions for GC, GCxGC, µGC, GC-AED, GC-MS, GC-QQQ, LC, LC-MS, LC-QQQ and Q-TOF LC-MS applications.
JAS serves key industries such as
Chemical•Environmental•FoodandFlavor•Forensic•MechanicalEngineering•Petrochemical•Pharmaceutical•
JAS Products for GC
AtomicEmissionDetector•CryoTrap•CustomizedValvingSystem•EzPrep-PreparativeFractionCollector•Olfactometer•Scotti-RFIDSystems•UNISInlets•
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