Eliminating Molecular Interferences in ICP-MS for the Simplest Method Development Dr. Torsten Lindemann.

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Presentation transcript:

Eliminating Molecular Interferences in ICP-MS for the Simplest Method Development Dr. Torsten Lindemann

What are Molecular Interferences ? Isotope Interference 31P 15N16O 14N16OH 30Si1H 12C19F 47Ti 32S15N 33S14N 1H32S14N 52Cr 40Ar12C 36Ar16O 36S16O 1H234S16O 56Fe 40Ar16O 40Ca16O 28Si2 60Ni 44Ca16O 23Na37Cl 23Na214N 28Si32S 75As 40Ar35Cl 40Ca35Cl Molecular species which occur at the same nominal mass as the analyte: Formed in the plasma and/or interface Originate from the matrix and the Ar plasma gas Matrix dependent Plasma condition dependent

Quadrupole and Sector Field Mass Spectrometers Quadrupole: Sector Field: +ve DC +ve RF -ve DC -ve RF Unit Resolution High Resolution Collision / Reaction Cell necessary R=m/Δm

iCAP Q Quadrupole ICP-MS: QCell with Flatapole for Interference Removal SEM with > 9 orders of linear dynamic range and long lifetime Thermo Scientific™ iCAP™ Q Quadrupole ICP-MS Quadrupole mass analyzer QCell with Flatapole for improved ion transmission and reliable interference reduction with He KED and reaction cell chemistry (non-consumable) Cones & Lenses: easily accessible RAPID lens for efficient removal of neutral species (maintenance-free)

iCAP Q Quadrupole ICP-MS: QCell with Flatapole for Interference Removal SEM with > 9 orders of linear dynamic range and long lifetime Thermo Scientific™ iCAP™ Q Quadrupole ICP-MS Quadrupole mass analyzer QCell with Flatapole for improved ion transmission and reliable interference reduction with He KED and reaction cell chemistry (non-consumable) Cones & Lenses: easily accessible RAPID lens for efficient removal of neutral species (maintenance-free)

High Resolution ICP-MS ELEMENT 2 Electrostatic Analyzer Ion Detection Magnet Interface (sampler & skimmer) @ ground potential 8 kV Ion Acceleration & Focusing Ion Production

40Ar35Cl Interference on 75As m/z 40 + 35 40Ar35Cl 75 75As m/z 75

Small Mass Difference Between 75As and 40Ar35Cl m/z 39.962 + 34.969 40Ar35Cl 74.931 75As m/z 74.921

Resolution to Resolve Interferences LR HR 5 µm MR 16 µm Resolution R = m/Δ m LR: Low Resolution: R ≥ 300 MR: Medium Resolution: R ≥ 4 000 HR: High Resolution: R ≥ 10 000 It takes < 1 s to change resolution The slit width defines the ion beam entering the magnetic field Narrower slits are used for higher resolution

As in Low Resolution 75As? Low Resolution

As in Low Resolution 75As? Low Resolution

As in Medium Resolution

As is Resolved from ArCl in High Resolution m/z 74.9307 75As m/z 74.9211

As Quantification: We Measure only As High Resolution 75As m/z 74.9211

P in 1000 mg/L Si / 3% HF / 2% HNO3

P in 1000 mg/L Si / 3% HF / 2% HNO3 (MR) 12C19F Medium Resolution 30Si1H 1H14N16O 31P

Interferences in 1000 ppm Si / 3% HF / 2% HNO3 (MR) 28Si16O 29Si18O 28Si19F 12C16O2 44Ca 47Ti ? 35Cl16O 40Ar12C 36S16O 36Ar16O 1H230Si19F 52Cr ? 51V

Interferences in 1000 ppm Si / 3% HF / 2% HNO3 (MR) ? 28Si2 40Ar16O 28Si30Si ? ? 56Fe 58Ni 29Si16O18O 28Si19F2 28Si35Cl 28Si38Ar 66Zn 63Cu ? ?

P Calibration in 1000 ppm Si: 1, 5, 10, 50, 100, 500 ppt 4400 cps / ppb P 6 ppt LoD 70 ppt BEC

1:10 Diluted Seawater: Removal of Interferences in Medium Resolution

1:10 Diluted Seawater: Removal of Interferences in Medium Resolution 31P16O 15N16O2 35Cl16O 34S16O1H 47Ti 51V 52Cr 40Ar12C 40Ca12C 36S16O 35Cl17O 40Ar15N 55Mn ?

1:10 Diluted Seawater: Removal of Interferences in Medium Resolution 42Ca16O1H 43Ca16O 23Na36Ar 40Ar18O1H 40Ar16O 40Ca16O 44Ca12C ? 56Fe 59Co 60Ni 44Ca16O 23Na40Ar ? ? 63Cu

Ti in 10 % H2SO4

33S14N 47Ti ? Ti in 10 % H2SO4 (MR) Medium Resolution 4000 cps / ppb Ti 0.2 ppt LoD 0.77 ppt BEC ?

52Cr 36S16O ? Cr in 10 % H2SO4 (MR) Medium Resolution 53000 cps / ppb Cr 0.15 ppt LoD 0.5 ppt BEC ?

Figures of Merit P Ti Cr Matrix 1000 ppm Si / 3 % HF / 2 % HNO3 10 % H2SO4 Sensitivity 4400 cps/ppb 4000 cps/ppb 53000 cps/ppb Background Equivalent Concentration 70 ppt 0.77 ppt 0.5 ppt Limit of Detection 6 ppt 0.2 ppt 0.15 ppt

Conclusions With Sector Field ICP-MS it is not necessary for the analyst to have any information about the sample or the expected interferences before analysis. Just dilute and shoot. All interferences are simply separated and observed by conducting a survey scan with an increased mass window. Methods can be defined with isotopes to be analyzed in different resolution settings with switching times between resolutions ≤ 1 s. This allows fast sample throughput without sacrificing the multielemental capabilities of ICP-MS. High mass resolution provides visual, simple and unequivocal data confidence. This confidence in the accuracy of the results makes Sector Field ICP-MS the ideal tool for applications where indisputable results are required. This is the reason why Sector Field ICP-MS is used in many regulatory and metrology institutions.