Results and Discussion
The performance of the ISQ 7610 system was evaluated using sixteen replicate injections of a 10 fg/µL OFN standard in iso-octane. Stable peak area responses were observed with %RSD of <7% as reported in Figure 1. The minimum %RSD calculated using n=8 injections was 5.7, and it was used to derive the IDL that resulted = 1.7 fg on column. Figure 2 shows the overlaid chromatograms of the injections that were used to derive the IDL. To verify the IDL, a standard of OFN at 2 fg was injected. As demonstrated in Figure 3, shows the OFN peak was clearly detected at such low concentration with a peak-to-peak calculated S/N of 4:1.
%RSD=7
5000 4500 4000 3500 3000 2500 2000 1500 1000 500
Figure 1. Absolute peak area responses over 16 injections.
6.5e3 8.0e3
6.5e3 8.0e3
4.5e3 6.0e3
5.5e3 7.0e3
3.5e3 5.0e3
6.5e3 8.0e3
4.5e3 6.0e3
5.5e3 7.0e3
3.5e3 5.0e3
1.5e3 3.0e3
2.5e3 4.0e3
0.0e0 1.0e3
5.0e2 2.0e3
Figure 2. Overlaid chromatograms of eight consecutive injections of OFN at 10 fg on column showing a peak area %RSD=5.7. The calculated IDL is 1.7 fg. 7.5e3 counts
1.5e3 3.0e3
2.5e3 4.0e3
The ISQ 7610 off-axis ion source, the unique s-shaped ion-guide, and the Thermo Scientifi c™ XLXR™ detector allowed for improved instrument performance. The off-axis ion source and unique s-shaped ion-guide creates a curved path, which allows chemical and neutral noise to be kept to a minimum, enabling lower detection limits. The XLXR detector provides the sensitivity to detect and amplify the low number of transmitted ions needed at this challenging analyte concentration.
0.0e0 1.0e3
5.0e2 2.0e3
RT: 3.863 – OFN min
4.5e3 6.0e3
5.5e3 7.0e3
7.5e3 counts
3.5e3 5.0e3
1.5e3 3.0e3
2.5e3 4.0e3
0.0e0 1.0e3
5.0e2 2.0e3
min 7.5e3 counts
5000 4500 4000 3500 3000 2500 2000 1500 1000 500
RT: 3.863 – OFN
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Injection number
RT: 3.863 – OFN
5000 4500 4000 3500 3000 2500 2000 1500 1000 500
%RSD=7
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Injection number
2.6e3 2.5e3 2.4e3 2.3e3 2.1e3 2.0e3 1.9e3 1.8e3 1.6e3 1.5e3 1.4e3 1.3e3 1.1e3 1.0e3 8.8e2 7.5e2 6.3e2 5.0e2 4.0e2
2.8e3 2.8e3
1.5e3 1.4e3 1.3e3 1.1e3 1.0e3 8.8e2 7.5e2 6.3e2 5.0e2 4.0e2
counts
RT: 3.865 – OFN min 25
AS 1610 autosampler Syringe
Injection volume
AS 1610 autosampler Syringe
Pre-injection solvent and cycles None Sample rinses
2.6e3 2.5e3 2.4e3 2.3e3 2.1e3 2.0e3 1.9e3 1.8e3 1.6e3 1.5e3 1.4e3 1.3e3 1.1e3 1.0e3 8.8e2 7.5e2 6.3e2 5.0e2 4.0e2
2.8e3 2.8e3
Injection volume
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Injection number
%RSD=7 Column
Post-injection solvent and cycles None TRACE 1610 GC system
Pre-injection solvent and cycles None Sample rinses
Conclusion ColumnSSL mode Liner
AS 1610 autosampler Syringe
Liner
Injection volume Inlet temperature
Split flowReferences Splitless time
5
Post-injection solvent and cycles None TRACE 1610 GC system
10 µL, 25 gauge, 50 mm length, cone tip (P/N 36500525)
5
Figure 3. Chromatogram of 2 fg OFN on-column with a signal-to-noise ratio of 4 to 1. 1 µL
Thermo Scientific™ TraceGOLD™
The ISQ 7610 system with the ExtractaBrite ion source exhibits low instrument detection limits, ensuring confi dence in trace analysis. The use of a statistical method to determine the IDL demonstrates the consistent and sensitive detection that can be achieved at this challenging analyte concentration. The detection limits using a 10 fg on-column amount have been shown to be highly reproducible. The exceptionally sensitive XLXR detector, complemented by the innovative s-shaped ion guide, effectively reduces noise while maintaining maximum sensitivity, leading to OFN IDLs signifi cantly below 5 fg on column.
TG-5MS 30 m × 0.25 mm × 0.25 µm (P/N 26098-1420)
TG-5MS 30 m × 0.25 mm × 0.25 µm (P/N 26098-1420) 220 ˚C
Thermo Scientific™ TraceGOLD™ Splitless
1 µL
Pre-injection solvent and cycles None Sample rinses
5 SSL mode
Split flow Column
Liner
Inlet temperature Carrier flow
Splitless time
Post-injection solvent and cycles None TRACE 1610 GC system
Septum purge flow Oven program
2. International Union of Pure and Applied Chemists (IUPAC),
http://media.iupac.org/publications/analytical_ compendium/Cha18sec437.pdf
Splitless 220 ˚C
Constant flow of 5.0 mL/min Constant He flow of 1.2 mL/min
To request a technical note titled Determination of the instrument detection limit of the TSQ 9610 triple quadrupole GC-MS/MS with Advanced Electron Ionization (AEI) source, please contact: CMD.APACMarketing@thermofi
sher.com
50 mL/min 0.5 min
Septum purge flow Find out more at thermofi
sher.com/ISQ7610 Carrier flow
ISQ 7610 GC-MS system MS transfer line temperature OvIeon source temperature Ionization mode
n pr gram SSL mode
ISQ 7610 GC-MS system MS transfer line temperature Ion source temperature Ionization mode Emission current
Inlet temperature Emission current
Split flow Scan start
Splitless time Scan mode
New Quadrupole Analysers for Vacuum Process Analysis Scan start min
Carrier flow
Scan mode Dwell time
Septum purge flow Dwell time
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Hiden Analytical introduce the HPR-30 Series quadrupole analysers for vacuum process analysis. The Hiden HPR-30 Series are bolt on vacuum process analysers designed for fast response, high sensitivity analysis of gas and vapour species. Equipped with Hiden’s multi-level software package, offering simple control of mass spectrometer parameters and complex manipulation of data and control of external devices. Applications include leak detection, contamination monitoring, process trend analysis and analysis of high mass species and precursors used in ALD and MOCVD.
Detector gain Oven program
Detector gain Standard mass range is 200 amu, versions up to 1000 amu are offered.
Optional upgrades include the innovative Hiden 3F series triple fi lter quadrupole system providing enhanced abundance sensitivity, part-per-billion (ppb) detection levels and high contamination resistance, particularly suited to the analysis of aggressive gases in CVD and RIE applications. Standard mass range is 200 amu, versions up to 1000 amu are offered.
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Multiple sampling confi gurations are offered to suit a full range of process pressure and vacuum system geometry requirements. Versions are offered with single, or multiple sampling inlets, either unheated or heated to allow sampling of volatile species.
Systems are offered cart mounted, and with height adjustment for maximum compatibility between tools. For pulsed deposition processes, time resolved measurements are offered to 50 ns time resolution.
More information online:
ilmt.co/PL/Xke0 56988pr@reply-direct.com
The HPR-30 Series are designed to offer a fully featured, fl exible and powerful solution for the monitoring of parameters in all aspects of process gas analysis such as leak detection, vacuum quality and precursor monitoring.
ISQ 7610 GC-MS system MS transfer line temperature Ion source temperature Ionization mode Emission current Scan start Scan mode Dwell time
Detector gain
SIM m/z 272 0.1 s
1.00E+06 Thermo Scientific™ TraceGOLD™
Constant flow of 5.0 mL/min Constant He flow of 1.2 mL/min
45 ˚C (0.5 min), 40 ˚C/min to 190 ˚C (0 min)
250 ˚C 200 ˚C
Splitless EI
Read, Share and Comment on this Article, visit:
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250 ˚C 200 ˚C EI
50 µA
220 ˚C 50 µA
50 mL/min 3.10 min
0.5 min SIM m/z 272
Constant flow of 5.0 mL/min 0.1 s
3.10 min1.00E+06 SIM m/z 272 0.1 s
1.00E+06
250 ˚C 200 ˚C EI
50 µA 3.10 min Constant He flow of 1.2 mL/min
45 ˚C (0.5 min), 40 ˚C/min to 190 ˚C (0 min)
TG-5MS 30 m × 0.25 mm × 0.25 µm (P/N 26098-1420)
45 ˚C (0.5 min), 40 ˚C/min to 190 ˚C (0 min)
Splitless Liner single taper with wool, 4 mm ID, 78.5 mm length (P/N 453A0924)
1. U.S. Code of Federal Regulations, 49 FR 43430, (Oct. 26, 1984); 50 FR 694, 696 (Jan. 4, 1985), as amended at 51 FR 23703 (June 30, 1986),
http://www.ecfr.gov/cgi-bin/text-idx?SID=efe93db42854f88dffcf 66ba8de737e6&mc=true&node=ap40.23.136_17.b&rgn=div9
Splitless Liner single taper with wool, 4 mm ID, 78.5 mm length (P/N 453A0924)
50 mL/min 0.5 min
10 µL, 25 gauge, 50 mm length, cone tip (P/N 36500525)
Splitless Liner single taper with wool, 4 mm ID, 78.5 mm length (P/N 453A0924)
counts
RT: 3.865 – OFN min
10 µL, 25 gauge, 50 mm length, cone tip (P/N 36500525)
1 µL min
08/03/2022 10:41
08/03/2022 10:41
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WWW.LABMATE-ONLINE.COM
08/03/2022 10:41
3.80 3.81 3.82 3.80 3.80 3.81 3.82 3.80 3.81 3.82 3.83 3.84 3.85 3.80 3.81 3.82 3.83 3.84 3.85 3.86 3.87 3.88 3.89 3.90 3.91 3.92 3.93 3.86 3.87 3.88 3.89 3.90 3.91 3.92 3.93 3.83 3.84 3.85 3.86 3.87 3.88 3.89 3.90 3.91 3.92 3.93 3.80 3.81 3.82 3.83 3.84 3.85 3.86 3.87
3.88 3.89 3.90 3.91
3.92 3.93
3.81 3.82 3.83 3.84 3.85 3.86 3.87
3.88 3.89 3.90 3.91
3.83 3.84 3.85 3.86 3.87
3.88 3.89 3.90 3.91
3.92 3.93
3.92 3.93
Peak area, counts*s
Peak area, counts*s
Peak area, counts*s
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