ICP-MS : The Ultimate GC Detector
Mina Tanoshima, Steve Wilbur, and Emmett Soffey
Agilent Technologies Inc . 34th International Symposium on Capillary Chromatography 2010
Experimental
Introduction
Gas chromatography (GC) is widely ud for the speciation and detection of volatile organic compounds in many applications and industries. There are many detectors for GC, such as PFPD/FPD ((puld) flame photometric detector) or SCD (Sulfur chemiluminescence detector) for sulfur, NPD (nitrogen/phosphorus detector) for nitrogen and phosphorus and ECD (electron capture detector) for the halogens. GC is also combined with a mass spectrometer or mass lective detector (MS or MSD), both with single quadrupole or triple-quad (QQQ). However, none of the detectors is capable of providing universal, element specific quantification in the manner of ICP-MS. ICP-MS provides a unique combination of rapid multi-element/isotope analysis, with very high nsitivity.
Results and Discussion
Conclusions
Figure 1. Agilent’s ICP -MS coupled to the Agilent’s 7890A GC.
Instrumentation
Agilent’s 7890A GC and Agilent’s 7700x ICP -MS were connected using the new GC interface kit provided by Agilent (As shown in Figure 1.) to evaluate the three analys; 1)Organo-tin, 2) Polybrominated Diphenyl Ether (PBDE), and 3) Sulfur species in diel. This GC interface connects the two instruments via a passivated, heated Sulfinert ®tube 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 is shown in Figure 2.
The u of ICP-MS as a GC detector significantly extends GC capability and expands its application. With a well-designed GC / ICP-MS interface featuring high
temperature and inertness, Organo-tin , PBDE and sulfur compounds in diel were successfully analyzed.
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Tho results demonstrated benefit of ICP-MS’ ultimate detection limit and multi element analysis capability.
1) Organo-tin analysis亲爱的英文单词
The toxic effects of organo-tin compounds in the environment are well known and rearch has begun to include matrices with human health implications, such as afood, manufactured products, and human blood samples. In this study, a mixed organo-tin standard was analyzed. The analysis was completed in less than 12 minutes achieving detection limit of 5.9ppt for tributyl tin (TBT).
GC Injection Splitless 1ul
Column
DB-5MS (5m x 0.25 mm x 0.25um film thickness)Oven Program
80℃(1min), 20℃/min -> 320℃(5min)Carrier gas He at 7mL/min Inlet Temp 260 deg C Transfer line temp
250 deg C
ICP injector temp 280 deg C
ICP-MS ICP-MS model 7700x RF Power 1250 W Sample Depth 7 mm Carrier gas 0.61 L/min Aux Gas 1.5 L/min Additional Gas No Monitored mass (m/z)
79, 81
to是什么意思>大雁塔 英文GC Injection Splitless 1ul
Column HP-5 (30m x 0.32mm i.d. x 0.25 um film thickness)
Oven Program
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70 deg(1min) ~ 30deg/min ~190deg (0min) ~ 15deg/min ~ 270deg (4min)Carrier gas He at 2mL/min Inlet Temp 290 deg C Transfer line temp 250 deg C ICP injector temp
250 deg C
ICP-MS ICP-MS model 7700x
RF Power 1200 W
Sample Depth 8 mm Carrier gas 0.80 L/min Aux Gas 1.5 L/min Additional Gas
No
Monitored mass (m/z)
118,120
2) Polybrominated Diphenyl Ether (PBDE) analysis
indicatePBDEs are widely ud flame retardants added to many common houhold products, such as mattress and furniture, and electronic devices. However their similarity in structure to PCBs and dioxins has raid concerns about health risks associated with their u. For this study, a PBDE mix(CIL Predominant Congener Mixture EO-5103) containing 14 different PBDEs were analyzed. (Chromatogram is shown in Figure 4.) All the PBDEs were parated successfully with good nsitivity, even for the difficult #209 (decaBDE) congener, which is thermally labile and
儿童情商decompos easily during GC paration. The detection limit was150ppt for Deca BDE .
3) Sulfur analysis in diel fuel
Sulfur in motor fuels has been implicated in global warming and acid rain. It is also a catalyst poison for automobile catalytic converters and refinery catalytic crackers. Reducing total sulfur in motor fuels has become a critical air pollution control goal worldwide. Figure5 show the chromatogram for low sulfur in diel samples (NIST 2724B).GC and ICP-MS operating parameters are shown in Table 3.
Figure 2. Schematic diagram for Agilent’s GC -MS interface for the 7890GC/7700 ICP-MS
RT (min)
C o u n t
Full Time Range EIC (mass 79)
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C o u n t
Full Time Range EIC (mass 120):
RT (min)
Figure 4. Chromatogram of mixed PBDE standard: 25ppb each compound except #138 (37.5ppb) and #209 (100ppb)
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Figure 3. Chromatogram of 10ppb Organo-tin standard. The samples was delivaized beforehand. Table 1. Method parameters for the paration of Organo-tin using the GC with ICP-MS detection.
(1) 2, 2’,4-TriBDE (BDE –17)
(2) 2, 4’,4-TriBDE (BDE –28)
美语(3) 2, 3’,4’,6-TetraBDE (BDE –71)
(4) 2, 2’,4,4’-TetraBDE (BDE –47)
(5) 2, 3’,4,4’-TetraBDE (BDE –66) (6) 2, 2’,4,4’,6-PentaBDE (BDE –100) (7) 2, 2’,4,4’-5-PentaBDE (BDE –99) (8) 2, 2’,3,4,4’-PentaBDE (BDE –85) (9) 2, 2’,4,4’,5,6’-HexaBDE (BDE –154) (10) 2, 2’,4,4’,5,5’-HexaBDE (BDE –153)
(11) 2, 2’,3,4,4’,5’-HexaBDE (BDE –138) (12) 2, 2’,3,4,4’,5’,6-heptaBDE (BDE –183) (13) 2, 3,3’,4,4’,5’,6’-HeptaBDE (BDE –190) (14) DecaBDE (BDE –209) Table 2. Method parameters for the paration of PBDEs using the GC with ICP-MS detection.
GC Injection Split 1:50 1ul
Column HP-5 (30m x 0.32mm i.d. x 0.25 um film thickness)
Oven Program 40deG(4min) ~ 20deG/min ~250deG (1min)Carrier gas He at 2.5mL/min Inlet Temp 250 degC Transfer line temp 250 degC ICP injector temp
260 degC
ICP-MS ICP-MS model 7700x RF Power 1550 W Sample Depth 8 mm Carrier gas 0.80 L/min Aux Gas 1.5 L/min Additional Gas No Monitored mass (m/z)
118,120
Table 3. GC and ICP-MS operating parameters.
Figure 5. Carbon and sulfur extracted ion chromatograms for NIST 2724B low sulfur.RT (c)
C o u n t
