Results and Discussion: ICP-MS: The Ultimate GC Detector
Results and Discussion: ICP-MS: The Ultimate GC Detector
Mina Tanoshima, Steve Wilbur and Emmett Soffey , Agilent Technologies Inc.
nitrogen and phosphorus and ECD (electron capture detector) for the halogens. GC study, a mixed organo-tin standard was analyzed. The analysis was completed Column DB-5MS (5m x 0.25 mm x
0.25um film thickness)
RF power 1250 W
is also combined with a mass spectrometer or mass selective detector (MS or MSD), in less than 12 minutes achieving detection limit of 5.9 ppt for tributyl tin (TBT). Oven program 80℃ (1min), 20℃/min -> 320℃ Sample depth 7 mm
both with single quadrupole or triple-quad (QQQ). However, none of these detectors (5min)
Carrier gas 0.61 L/min
is capable of providing universal, element specific quantification in the manner of Carrier gas He at 7mL/min
Full Time Range EIC (mass 120): Inlet temp 260 deg C
ICP-MS. ICP-MS provides a unique combination of rapid multi-element/isotope Aux gas 1.5 L/min
Count
Experimental
3) Sulfur analysis in diesel fuel
Sulfur in motor fuels has been implicated in global warming and acid rain. It is also
Instrumentation
a catalyst poison for automobile catalytic converters and refinery catalytic crackers.
An Agilent 7890A GC and Agilent 7700x ICP-MS were connected using the new
Reducing total sulfur in motor fuels has become a critical air pollution control goal
Agilent GC-ICP-MS interface (Figure 1) to evaluate these three analyses; 1)Organo- RT (min) worldwide. Figure 5 show the chromatogram for low sulfur in diesel samples
tin, 2) Polybrominated Diphenyl Ether (PBDE), and 3) Sulfur species in diesel. The
(NIST 2724B). GC and ICP-MS operating parameters are shown in Table 3.
interface connects the two instruments via a passivated, heated Sulfinert ® tube
Figure 3. Chromatogram of 10 ppb organo-tin standard. The samples was derivatized beforehand
between the GC column and the tip of the ICP injector using a special torch with a
heated injector to maintain constant high temperature and inertness. The schematic
Table 1. Method parameters for the separation of organo-tin using the GC with ICP-MS detection
is shown in Figure 2.
GC ICP-MS
Count
um film thickness)
RT (sec)
concerns about health risks associated with their use. For this study, a Injection Split 1:50 1ul ICP-MS model 7700x
PBDE mix(CIL Predominant Congener Mixture EO-5103) containing 14 Column HP-5 (30m x 0.32mm i.d. x 0.25
um film thickness)
RF power 1550 W
different PBDEs were analyzed. (Chromatogram is shown in Figure 4.) All Oven program 40deG(4min) ~ 20deG/min
Sample depth 8 mm
~250deG (1min)
Figure 1. Agilent 7700x ICP-MS coupled to an Agilent 7890A GC the PBDEs were separated successfully with good sensitivity, even for the Carrier gas 0.80 L/min
Carrier gas He at 2.5mL/min
difficult #209 (decaBDE) congener, which is thermally labile and Inlet temp 250 degC
Aux gas 1.5 L/min
decomposes easily during GC separation. The detection limit was150 ppt Transfer line temp 250 degC
Additional gas No