Thermo Scientific DFSapps.thermoscientific.com/media/SID/IOMS/PDF/...19 Peakshape (separation)...
Transcript of Thermo Scientific DFSapps.thermoscientific.com/media/SID/IOMS/PDF/...19 Peakshape (separation)...
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Thermo Scientific DFSHigh Resolution Sector Field MS
Dual Data Acquisition on a DFS
Heinz Mehlmann, Thermo Fisher, Bremen, Germany
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Dual Data Acquisition
- Hardware
- Theoretical Background
- Performance
- Realisation
Dual GC single MS wide AS configuration
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first peak last peak
Typical dioxin GC run on a 60m column
The first and last peak of a chromatogram defines the section of analytical intrest.
Theoretical Background
section of analytical interestwasted time wasted time
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GC 1
GC 2
sequence timescale in normal mode
sample 1 sample 3
Theoretical Background
sample 2
Dual GC-MS systemSingle GC-MS system
No timesaving.
Why?
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Theoretical Background
Both columns are directed into the source.
column GC 1 column GC 2
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GC 1
GC 2
GC 1
GC 2
sequence timescale in normal mode
sequence timescale with DUAL DATA Aquisition.
sample 1
sample 2
sample 3
sample 1
sample 2
sample 3
sample 4
sample 5
sample 6
Theoretical Background
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Theoretical Background
Continuous Dataflow
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The following sample in the sequence will be injected during aquisition of the previous GC run.
Realisation
GC 1
GC 2
Sequence timescale with DUAL DATA Aquisition.
A hardware based modification is necessary.
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Dynamic Flow Switching System
Realisation
A staggert injection can be realised with a hardware based modification in each GC.
Injector
analytical columnT-connector
swiching
valves
to MS
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Dynamic Flow Switching System
The column-flow is directed into the MS.
The column-flow is directed into the service vacuum
and He compensates the flow into the ionsource.
Realisation
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Cutout of a high conc. sample
Realisation
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Cutout of solventpeaks
Realisation
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Dynamic Flow Switching System
Hardware
Transfereline
Injector
Analytical Column
He
Vacuum
T-Connector
soldered stainless steel capillary
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Dynamic Flow Switching System
Hardware
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Dynamic Flow Switching System
DFS
Column
Hardware
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GC 1
GC 2
DFS
Time
GC 1 GC 2GC 2GC 1
Principle
Timing
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Sample: 1µl CS3 / CPM 8290/1613; Column: Thermo TR-Dioxin 60m x 0.25mm ID x 0.1µm film; Oven: 150 (2)-25-230(25)-6-320(6)
Performance PCDF/PCDD
native TCDF (303.9010 m/z)
native TCDF (305.8913 m/z)
13C12 Standard TCDF (315.9413 m/z)
13C12 Standard TCDF (315.9413 m/z)
RT: 20.16 - 31.84 :
21 22 23 24 25 26 27 28 29 30 31
Time (min)
50
100
50
100
50
100
50
100
50
100
Rela
tive A
bundance
50
100
50
100
50
10020.88
27.1731.08
25.75
20.88
27.1631.08
25.77
27.12
27.12
23.0730.6928.7128.42
28.1227.52
23.0730.6928.7128.42
28.1127.52
28.6627.49
28.6627.49
NL: 5.31E4
m/z= 303.8716-303.9324 MS DioxFur_5w_01_090316165536
NL: 6.78E4
m/z= 305.8684-305.9296 MS DioxFur_5w_01_090316165536
NL: 3.96E5
m/z= 315.9104-315.9736 MS DioxFur_5w_01_090316165536
NL: 5.01E5
m/z= 317.9072-317.9708 MS DioxFur_5w_01_090316165536
NL: 3.18E4
m/z= 319.8650-319.9290 MS DioxFur_5w_01_090316165536
NL: 4.24E4
m/z= 321.8618-321.9262 MS DioxFur_5w_01_090316165536
NL: 2.50E5
m/z= 331.9038-331.9702 MS DioxFur_5w_01_090316165536
NL: 3.19E5
m/z= 333.9006-333.9674 MS DioxFur_5w_01_090316165536
native TCDD (319.8960 m/z)
native TCDD (321.8930 m/z)
13C12 Standard TCDD (331.9363 m/z)
13C12 Standard TCDD (333.9333 m/z)
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Sample: 1µl CS3 / CPM 8290/1613; Column: Thermo TR-Dioxin 60m x 0.25mm ID x 0.1µm film; Oven: 150 (2)-25-230(25)-6-320(6)
Performance PCDF/PCDD
native HxCDF (373.8202 m/z)
native HxCDF (375.8172 m/z)
13C12 Standard HxCDF (383.8633 m/z)
13C12 Standard HxCDF (385.8604 m/z)
native HxCDD (389.8151 m/z)
native HxCDD (391.8121 m/z)
13C12 Standard HxCDD (401.8554 m/z)
13C12 Standard HxCDD (403.8524 m/z)
RT: 38.44 - 43.53
38.5 39.0 39.5 40.0 40.5 41.0 41.5 42.0 42.5 43.0 43.5
Time (min)
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50
100
0
50
100
0
50
100
0
50
100
0
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100
Rela
tive A
bundance
0
50
100
0
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100
0
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10039.39 41.8841.1641.01
42.91
41.8841.1639.39 41.01 42.89
41.8641.1440.99 42.89
41.8641.1440.99 42.88
40.16 42.5142.19
40.16 42.19 42.5142.08
42.18 42.4942.06
42.18 42.4942.06
NL: 5.27E5
m/z= 373.7836-373.8584 MS DioxFur_5w_01_090316165536
NL: 4.28E5
m/z= 375.7804-375.8556 MS DioxFur_5w_01_090316165536
NL: 5.76E5
m/z= 383.8042-383.8810 MS DioxFur_5w_01_090316165536
NL: 1.07E6
m/z= 385.8216-385.8988 MS DioxFur_5w_01_090316165536
NL: 3.87E5
m/z= 389.7770-389.8550 MS DioxFur_5w_01_090316165536
NL: 3.06E5
m/z= 391.7738-391.8522 MS DioxFur_5w_01_090316165536
NL: 7.43E5
m/z= 401.8158-401.8962 MS DioxFur_5w_01_090316165536
NL: 5.95E5
m/z= 403.8126-403.8934 MS DioxFur_5w_01_090316165536
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Peakshape (separation)
Performance Peakshape
The separation of 2,3,7,8-TCDD
from most closely eluted isomers
is below 25% Valley, according to
EPA 1613.
2,3,7,8-TCDD
< 25%
Sample: 1µl CS3 / CPM 8290/1613; Column: Thermo TR-Dioxin 60m x 0.25mm ID x 0.1µm film; Oven: 150 (2)-25-230(25)-6-320(6)
RT: 22.57 - 31.20
23 24 25 26 27 28 29 30 31
Time (min)
20
40
60
80
100
20
40
60
80
100
20
40
60
80
100
Rela
tive A
bundance
20
40
60
80
10023.07
30.6928.7128.42
28.1227.52
23.07
30.6928.7128.42
28.1127.52
28.6627.49
28.6627.49
NL:3.20E4
m/z= 319.8650-319.9290 MS DioxFur_5w_01_090316165536
NL:4.28E4
m/z= 321.8618-321.9262 MS DioxFur_5w_01_090316165536
NL:2.51E5
m/z= 331.9038-331.9702 MS DioxFur_5w_01_090316165536
NL:3.21E5
m/z= 333.9006-333.9674 MS DioxFur_5w_01_090316165536
native TCDD (319.8960 m/z)
native TCDD (321.8930 m/z)
13C12 Standard TCDD (331.9363 m/z)
13C12 Standard TCDD (333.9333 m/z)
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Sample: 1µl CS4-7474-62 CVS; Column: Restek Rtx@-1614 15m x 0.25mm ID x 0.1µm film; Oven: 120 (3)-10-300(6)
Performance PBDE
native TriBDE (405.8021 m/z)
native TBDE (485.7106 m/z)
native PeBDE (563.6311 m/z)
native HxBDE (643.5296 m/z)
native HpBDE (721.4401 m/z)
native DecBDE -2Br (799.3329 m/z)
native DiBDE (327.8916 m/z)
RT: 5.67 - 26.50
6 8 10 12 14 16 18 20 22 24 26
Time (min)
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100
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100
0
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100R
ela
tive A
bundance 0
50
100
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100
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50
1008.16 8.36
7.887.25
10.8311.25
10.31
9.66
13.6112.40
14.3715.64
15.77
17.24
15.6315.93
16.49 17.22
20.1117.96
19.73 20.23 21.79
18.08
21.7818.8921.99
19.0022.44
17.81 20.11
25.50
NL:7.60E5
m/z= 327.8815-327.9015 MS D90311A20
NL:4.34E5
m/z= 405.7981-405.8181 MS D90311A20
NL:3.09E5
m/z= 485.7010-485.7210 MS D90311A20
NL:3.47E5
m/z= 563.6120-563.6320 MS D90311A20
NL:3.93E5
m/z= 643.5200-643.5400 MS D90311A20
NL:1.97E5
m/z= 721.4310-721.4510 MS D90311A20
NL:1.97E4
m/z= 799.3230-799.3430 MS D90311A20
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Performance Deca BDE
RT: 24.56 - 26.33
24.6 24.8 25.0 25.2 25.4 25.6 25.8 26.0 26.2
Time (min)
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20
40
60
80
100
0
20
40
60
80
100
0
20
40
60
80
100
Rela
tive A
bundance
0
20
40
60
80
10025.49
25.49
25.49
25.49
NL:1.81E4
m/z= 799.2481-799.4079 MS D90311A20
NL:1.39E4
m/z= 801.2438-801.4041 MS D90311A20
NL:2.36E4
m/z= 811.2844-811.4467 MS D90311A20
NL:1.85E4
m/z= 813.2802-813.4428 MS D90311A20
13C12 Standard DecBDE -2Br (811.3732 m/z)
native DecBDE -2Br (799.3329 m/z)
native DecBDE -2Br (801.3309 m/z)
13C12 Standard DecBDE -2Br (813.3711 m/z)
Sample: 1µl CS4-7474-62 CVS; Column: Restek Rtx@-1614 15m x 0.25mm ID x 0.1µm film; Oven: 120 (3)-10-300(6)
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Sensitivity
1µl blood sample in the range of 20fg TCDD
Sample: 1µl Blood Sample; Column: Thermo TR-Dioxin 60m x 0.25µm x 0.1µm film; Oven: 120 (2)-10-220(10)-3-235(7)-4.6-310(1)
Performance Sensitivity
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Productivity
Performance Samplethrougput
Dual Data Acquisition
Increase of samplethrougput with no loss in performance.
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Dual Data AcquisitionTechnical Note
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Acknowledgment
Chuck Sueper Minneapolis /MN USA
Stefan Ahlbrand Altenberge Germany