Laser microprobe with fourier transform ion cyclotron resonance mass spectrometer for surface analysis.

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.

Complementary use of Fourier transform laser microprobe mass spectrometry and time-of-flight static secondary ion mass spectrometry for the study of the surface adsorption of organic dyes on silicate materials.

The adsorption of organic ionic dyes on different pore size engineered silica materials with potential application for industrial wastewater treatment has been investigated using Fourier transform laser microprobe mass spectrometry (FT-LMMS) and time-of-flight secondary ion mass spectrometry (TOF-S-SIMS). The complementary use of the two methods with different information depth allowed data on the subsurface distribution and pore penetration of the adsorbed organic compounds. Macroscopic methods were employed to determine the amount adsorbed on the particles and the specific external surface area. Local MS analysis allows identification of the organic dyes exclusively at the outer particle surface when the pore size is inferior to the size of the adsorbing molecule, or at the surface of the channels inside the material. Specifically, the monolayer information depth of TOF-S-SIMS causes a signal to refer essentially to the adsorbate at the outer particle surface, which is only a fraction of the total adsorption in mesoporous materials, while FT-LMMS allowed detection of the presence of adsorbates at the outer surface as well as inside the subsurface of 10 to 50 nm depending on the material under study. The observed data open perspectives for the molecular monitoring of the adsorption behaviour of different materials at the (sub) microm scale.