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Highlights from the 2016 Microscopy & Microanalysis Meeting in Columbus, OH. a New MS/MS Imaging Tof-SIMS Mass Spectrometer

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Highlights from the 2016 Microscopy & Microanalysis Meeting in Columbus, OH. a New MS/MS Imaging Tof-SIMS Mass Spectrometer By Shiladitya Chatterjee and Matthew R. Linford, Department of Chemistry and Biochemistry, Brigham Young University, Utah, USA Contributing Editors Highlights from the 2016 Microscopy & Microanalysis Meeting in Columbus, OH. A New MS/MS Imaging ToF-SIMS Mass Spectrometer, a Very Low Cost AFM, and a Remote Plasma Cleaning System e recently attended the 2016 (SE): Uniqueness Plots and Width Func- do not wish any vendors to feel like the Microscopy & Microanalysis tions in XPS, and Distance, Principal lack of an invitation to contribute to this W(M&M) meeting held at the Component, and Cluster Analyses in SE”. article is in any way a judgment of their Columbus Convention Center in Colum- These are topics we have recently pub- product. We are not trying to endorse bus, Ohio. Columbus is a beautiful, clean lished on in the Linford group.1-4 any products here. Finally, in the spirit of city. We arrived the Saturday before the Many of the sessions encouraged stu- our earlier articles, we hope to provide a conference and that evening attended a dent participation and there were a num- technical/tutorial view and commentary minor league baseball game (Columbus ber of student awards. In our experience, of the science and technology behind the Clippers). The home team won. Both pic- M&M 2016 drew an exceptional group of products we will be discussing. tures above are from the trip, and the pic- scientists and engineers. The next M&M ture of MRL was taken at the game. annual meeting will be in St. Louis, MO. v The M&M conference is an excellent We hope to see you there. meeting for anyone working in the fields In general when we go to conferences of microscopy, microanalysis, and thin we spend some time in the exhibition TOF-SIMS Parallel Imaging MS/MS film characterization. The conference ran hall. This is a great way to find out about Company: from July 24 – 28, 2016 and each day what’s new. Indeed, because our ability to featured 3 parallel sessions with topics synthesize and characterize many of the Physical Electronics such as advances in instrumentation and materials we work with depends on the (a division of ULVAC-PHI) microscopy in the biological and physical process and analytical tools at our disposal, Company Website: sciences. There were great posters in the thin film and material characterization are www.phi.com/physical-electronics.html evenings on a myriad of topics, including never far from advanced instrumentation. Company Contact: microfabrication, image processing, and Accordingly, we extended an invitation [email protected] nanomaterials. SC gave a poster entitled: to a few of the vendors at M&M 2016 to “Polyallylamine as an Adhesion Promoter provide us with information we might use Company Overview: for SU-8 Photoresist”. MRL gave an in- in a VT&C article. Three of them sent us According to the company, “Physical vited talk on “New Data Analysis Tools the content that we based this article on. Electronics (PHI) is a subsidiary of UL- for X-Ray Photoelectron Spectroscopy Of course we were not able to visit most VAC-PHI, the world’s leading supplier (XPS) and Spectroscopic Ellipsometry of the booths at the conference, and we of UHV surface analysis instrumentation 2 [email protected] September 2016 • Vacuum Technology & Coating used for research and development of becomes enormous. Today, analyses rou- by a 1 Da precursor selection window, is advanced materials in a number of high tinely produce secondary ion masses well accomplished by a 1.5 keV Collision-In- technology fields including: nanotech- over 2,000 m/z. Clearly, to further extend duced-Dissociation (CID) cell using Ar nology, microelectronics, storage media, the technique an advance is needed in the gas. Lateral resolutions produced in both bio-medical, and basic materials such as data acquisition of higher mass molecular MS1 and MS2 images were shown in the metals, polymers, and coatings. PHI’s ion fragments in order for TOF-SIMS to presented research to be < 200 nm. The innovative XPS, AES, and SIMS technol- reach its full potential for unambiguous MS2 fragment spectra from a sample of ogies provide our customers with unique compound identification and ease of data pure Crystal Violet demonstrates that the tools to solve challenging materials prob- interpretation. This is particularly import- 1 Dalton wide precursor selection win- lems and accelerate the development of ant for cellular and sub-cellular biological dow can eliminate or select 13C-contain- new materials and products.” tissue analysis, as well as micro-features ing precursor peaks, providing enhanced Product Description: on polymers, biomaterials and other or- MS2 data from samples with complex At the time of its introduction in the ganic materials. mixtures of additives on the surface. This 1980’s, Time-of-Flight Secondary Ion To provide this needed paradigm shift, data bodes well for imaging of lipids and Mass Spectrometry (TOF-SIMS) was Physical Electronics has designed a rev- metabolites from tissue samples. The principally a surface analysis research olutionary new TOF-SIMS Parallel Im- MS2 fragment ion spectra also demon- instrument. It provided elemental ion and aging MS/MS. Results from this unique strate better than 10 ppm mass accuracy 5 limited molecular fragment ion spectra and patented instrument were presented for the identified peaks. The conversion and images of the outer layers of solid ma- at the Microscopy and Microanalysis efficiency of precursor ion peaks to the terials. TOF-SIMS is based on the impact Conference in Columbus, Ohio – John spectrum of fragment ion peaks is, on av- of a finely focused, raster-scanned ion Hammond gave a talk on it. The newly erage, better than 10%. beam on the surface of the sample and the developed TOF-TOF tandem imaging A schematic of the PHI nanoTOF II time-of-flight mass analysis of the ejected mass spectrometer system allows con- imaging MS/MS is shown in Figure 1. The secondary ions (SIMS). Since its initial ventional TOF-SIMS (MS1) analysis and system design allows simultaneous MS successes, TOF-SIMS has evolved into a product ion (MS/MS or MS2) analysis to and MS/MS imaging up to 8 kHz, allowing more powerful technique for spectroscopy be acquired simultaneously and in par- MS1 and MS2 imaging and spectroscopy and imaging of molecular fragment ions. allel. Secondary ions for MS1 and MS2 in less than 15 minutes. Figure 2 shows This has been achieved, in part, by two or- analysis are produced from the same area a negative polarity MS2 spectrum of the ders of magnitude improvement in higher of the surface by a pulsed and digitally Erucamide polymer additive precursor mass ionization efficiencies. Improved raster-scanned primary ion nanoprobe. molecular ion. This spectrum allows the spatial focusing of the primary ion beams Activation of the precursor ions, defined structural identification of the location of has also improved the ultimate spatial res- olution observed for TOF-SIMS imaging of molecular fragment ions. All of these advances have expanded the breadth of applications, most nota- bly the use of TOF-SIMS for analyzing organic contamination, tissue cross sec- tions, pharmaceuticals, and polymer sur- faces with sub-micron spatial resolution. Nevertheless, the limitation of organic molecular fragment compositional peak assignments, based on TOF mass reso- lutions of up to 16,000 m/Δm and mass accuracies of ca. 10 to 20 ppm for current state-of-the-art TOF analyzers, has creat- ed ambiguity for many of the peak assign- ments above 200 m/z (for either positive or negative polarity ions). That is, there is uncertainty in peak assignments because the TOF mass spectrometers have tra- ditionally had good, but not great, mass resolution, and as the molecular weight of a fragment increases the number of pos- sible ways the elements can be combined Figure 1. Schematic of the Phi TOF-SIMS Imaging MS/MS instrument. Figure obtained and to make a fragment of the same mass used with permission from Phi (www.phi.com). Vacuum Technology & Coating • September 2016 www.vtcmag.com 3 Figure 2. MS/MS spectrum of the m/z 336 erucamide precursor ion. Figure obtained and used with permission from Phi (www.phi.com). the double bond. Figure 3 shows the MS1 images for a heat-treated polyethylene terephthalate film and the MS2 images from the positive polarity 577 m/z precursor ions. The simultaneous MS1 and MS2 imaging of the heat-treated PET sample confirmed that the crystal structure on the surface of the PET has a cyclic trimer structure. The MS1 images and MS2 images derived from the CID activation of the positive polarity 577 m/z precursor show that the crystal images are in exact registry with one another. Line scans (80% to 20% intensity) show <200 nm spatial resolution for both modes of imaging. Figure 4a shows the MS1 Figure 3. MS1 images and MS/MS (MS2) images from positive polarity m/z 577 precursor image for the granulomas in the cross- ions from a heat treated PET film. Figure obtained and used with permission from Phi section of the spleen of Zebrafish infected (www.phi.com). with Mycobacterium Marinum (a form of marine tuberculosis). Figure 4b and 4c show the elevated MS2 intensities of fatty acids (FA 16:0) around the granulomas, thought to be the result of metabolism of lipids in the macrophages trying to attack the infection in the granulomas. The spatial resolution of the elevated fatty acids observed in the MS2 image is 0.8 microns in Figure 4d.6 These results confirm that TOF-SIMS Imaging MS/MS can now provide easy and unambiguous molecular fragment ion peak identification and fast parallel imaging with MS1 and MS2 data.
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