Laser Microprobe with Fourier Transform Ion Cyclotron Resonance Mass Spectrometer for Surface Analysis

Abstract

Fourier transform ion cyclotron resonance laser microprobe mass spectrometry (FTICR LMMS) uses focused laser irradiation of solids with a spot of 5 microm and a FTICR mass analyzer for local analysis with high mass resolution. A new ion source design has been developed to improve the extraction and transfer of ions generated in an external laser microprobe source. Calculations predicted trapping of ions initially emitted with angles up to 40 degrees and 60 degrees from the surface and from a distance of 1 mm above the sample, respectively. The analytical performances of the method have been verified on two sets of test samples. First, detection of chemisorbed benzotriazole on copper, average of two monolayers, has been shown with less sample consumption than typically required in static secondary ion mass spectrometry with a time-of-flight analyzer. Second, experiments on a thermal plate for offset printing have shown the feasibility of analysis and quantification of dyes embedded in a polymer matrix.

Investigation of methods to enhance the secondary ion yields in TOF‐SIMS of organic samples

“…This solution contained 0.1% of an IR dye with a mass of 583 u (CAS No. 134127-48-3), [8] 0.8% of a blue dye with a mass of 469 u (CAS No. 2580-56-5), [8] and 14% novolak binder (Alnovol SPN452, Clariant, Germany).…”

“…134127-48-3), [8] 0.8% of a blue dye with a mass of 469 u (CAS No. 2580-56-5), [8] and 14% novolak binder (Alnovol SPN452, Clariant, Germany). This mixture was spin-coated onto test-grade silicon wafers, which were cleaned for 5 min by ultrasonification in methanol (Acros Organics, Belgium) and dried in a stream of hot air.…”

Atomic spectrometry update. Atomic mass spectrometry

“…Development of a new ion source and dedicated ion transfer optics allowed detection of a single monolayer with Fourier transform LMMS to be achieved with a 5 mm spot diameter. 162 Calculations predicted trapping of ions emitted initially at angles of up to 40 and 60 from the surface and from a distance of 1 mm above the sample, respectively. The improved analytical performance was demonstrated by the speciation of a copper complex present as a single monolayer.…”

Laser Ionization Mass Spectrometry at 55: Quo Vadis?

“…Technical details of the FT-LMMS setup and its applications have been published (Van Vaeck et al, 1994a, 1994b, and also discussed in Encyclopedia of Spectroscopy and Spectrometry (Van Vaeck & Adams, 1999). Several years ago, a new ion source was developed to improve the transport of ionized species into the FT-ICR mass analyzer (Moisio et al, 2007), but no new developments in the design of this instrument have been reported since then. Applications of this design will be reviewed in Chapter IV.…”