Time of flight secondary ion mass spectrometry, TOF-SIMS, is a highly surface sensitive analytical technique that provides information about composition with submicron lateral resolution. For select materials, TOF-SIMS provides unparalleled sensitivity along with excellent reproducibility, and as a mass spectrometric technique, it also provides excellent specificity. Of the analytical methods available, it is among the most surface sensitive, but the physical principles that underlie it are also the least understood. This volume describes the instrumentation, the physical principles behind the technique to the extent they are understood, and provides a practical approach for the interpretation of TOF-SIMS data. The use of advanced data processing methods such as multivariate statistics are described in a readily approachable manner. Given a basic background in undergraduate chemistry and physics, the book will be of use to any student with an interest in the technique.

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is the most versatile of the surface analysis techniques that have been developed during the last 30 years. This is the Second Edition of the first book ToF-SIMS: Surface analysis by Mass Spectrometry to be dedicated to the subject and the treatment is comprehensive

Chemical Imaging Analysis covers the advancements made over the last 50 years in chemical imaging analysis, including different analytical techniques and the ways they were developed and refined to link the composition and structure of manmade and natural materials at the nano/micro scale to the functional behavior at the macroscopic scale. In a development process that started in the early 1960s, a variety of specialized analytical techniques was developed – or adapted from existing techniques – and these techniques have matured into versatile and powerful tools for visualizing structural and compositional heterogeneity. This text explores that journey, providing a general overview of imaging techniques in diverse fields, including mass spectrometry, optical spectrometry including X-rays, electron microscopy, and beam techniques. - Provides comprehensive coverage of analytical techniques used in chemical imaging analysis - Explores a variety of specialized techniques - Provides a general overview of imaging techniques in diverse fields

Adhesives have been used for thousands of years, but until 100 years ago, the vast majority was from natural products such as bones, skins, fish, milk, and plants. Since about 1900, adhesives based on synthetic polymers have been introduced, and today, there are many industrial uses of adhesives and sealants. It is difficult to imagine a product—in the home, in industry, in transportation, or anywhere else for that matter—that does not use adhesives or sealants in some manner. The Handbook of Adhesion Technology is intended to be the definitive reference in the field of adhesion. Essential information is provided for all those concerned with the adhesion phenomenon. Adhesion is a phenomenon of interest in diverse scientific disciplines and of importance in a wide range of technologies. Therefore, this handbook includes the background science (physics, chemistry and materials science), engineering aspects of adhesion and industry specific applications. It is arranged in a user-friendly format with ten main sections: theory of adhesion, surface treatments, adhesive and sealant materials, testing of adhesive properties, joint design, durability, manufacture, quality control, applications and emerging areas. Each section contains about five chapters written by internationally renowned authors who are authorities in their fields. This book is intended to be a reference for people needing a quick, but authoritative, description of topics in the field of adhesion and the practical use of adhesives and sealants. Scientists and engineers of many different backgrounds who need to have an understanding of various aspects of adhesion technology will find it highly valuable. These will include those working in research or design, as well as others involved with marketing services. Graduate students in materials, processes and manufacturing will also want to consult it.

This book serves as a practical guide for applications of X-ray fluorescence spectrometry, a nondestructive elemental analysis technique, to the study and understanding of archaeology. Descriptions of XRF theory and instrumentation and an introduction to field applications and practical aspects of archaeology provide new users to XRF and/or new to archaeology with a solid foundation on which to base further study. Considering recent trends within field archaeology, information specific to portable instrumentation also is provided. Discussions of qualitative and quantitative approaches and applications of statistical methods relate back to types of archaeological questions answerable through XRF analysis. Numerous examples, figures, and spectra from the authors’ field work are provided including chapters specific to pigments, ceramics, glass, construction materials, and metallurgical materials.

The book provides an up-to-date overview of the fast growing area of Raman spectroscopy. The two-volume work describes how analytic methods using Raman spectroscopy allow for the chemical analysis of materials, providing even spatial resolution without precedent. In addition, external perturbations (strain, temperature, pressure) on molecules and their alignment can be analyzed. Raman spectroscopy can also provide information about the interactions of components, again at a high level of spatial resolution. In the form of tip-enhanced Raman spectroscopy (TERS), the method is a valuable tool for nanotechnology. This book is intended for researchers or lecturers in chemistry and materials science, who are interested in the composition and properties of their samples. It describes how Raman spectroscopy will enable them to examine thin layers, surfaces, and interfaces and improve their knowledge about the properties of composites. In addition, it can serve as a short introduction to vibrational spectroscopy.

Time of flight secondary ion mass spectrometric (ToF-SIMS) imaging is a powerful bioanalytical tool with the ability to produce molecular images of samples with submicron spatial resolution without the use of labels. In this thesis I will present the development of ToF-SIMS imaging methodology for biological analyses as well as applications that have yielded information about the role of lipids in membrane organization. In the first chapter, I introduce the plasma membrane and describe its fundamental role in maintaining life through the dynamic remodeling of its structure. I focus on two concepts that are believed to influence the localized chemical make up and structure of the membrane, intrinsic curvature and lipid domains. ToF-SIMS imaging is briefly described and a discussion of cluster ion bombardment and sample preparation is included. The chapter concludes with a survey of several important biological studies that have come out of the SIMS community. In Chapter 2 I report a protocol for the use of SIMS imaging to comparatively quantify the relative difference in cholesterol level between the plasma membranes of two cells. This development enables direct comparison of the chemical effects of different drug treatments and incubation conditions in the plasma membrane at the single-cell level. Relative, quantitative ToF-SIMS imaging was used to compare macrophage cells treated to contain elevated levels of cholesterol with respect to control cells. In-situ fluorescence microscopy with two different membrane dyes was used to discriminate morphologically similar but differentially treated cells prior to SIMS analysis. SIMS images of fluorescently identified cells reveal that the two populations of cells have distinct outer leaflet membrane compositions with the membranes of the cholesterol-treated macrophages containing more than twice the amount of cholesterol of control macrophages. Relative quantification with SIMS to compare the chemical composition of single-cells can provide valuable information about normal biological functions, causative agents of diseases, and possible therapies for diseases. Chapter 3 investigates prospects for three-dimensional SIMS analysis of biological materials using model multilayer structures and single cells. The samples were analyzed in a ToF-SIMS spectrometer equipped with a 20 and a 40 keV buckminsterfullerene (C60+) ion source. Specifically, molecular depth profile studies involving dehydrated dipalmitoylphosphatidylcholine (DPPC) organic films indicate that cell membrane lipid materials do not experience significant chemical damage when bombarded with C60+ ion fluences greater than 1015 ions/cm2. Moreover, depth profile analyses of DPPC?sucrose frozen multilayer structures suggest that biomolecule information can be uncovered after the C60+ sputter removal of a 20 nm overlayer with no appreciable loss of underlying molecular signal. The resulting depth information was used to characterize C60+ bombardment of biological materials. This information was used to controllably remove the plasma membrane of a single macrophage cell using a molecular depth profile approach allowing the analysis of the chemistry of the cytoplasm. Two methods that were developed to increase the reproducibility of biological SIMS analysis are covered in Chapter 4. First I demonstrate the utility of the C60+ cluster ion projectile for sputter cleaning biological surfaces to reveal obscured spatio-chemical information. Following the removal of nanometers of material from the surface using sputter cleaning; a frozen-patterned cholesterol film and a freeze-dried tissue sample were analyzed using ToF-SIMS imaging. In both experiments the chemical information was maintained after the sputter dose, due to the minimal chemical damage caused by C60+ bombardment. In fact, the damage to the surface produced by freeze-drying the tissue sample was found to have a greater effect on the loss of cholesterol signal than the sputter-induced damage. In addition to maintaining the chemical information, sputtering did not alter the spatial distribution of the surface chemistry. This approach removes artifacts that are common to many biological sample preparation schemes for ToF-SIMS imaging. Removing these artifacts, which may obscure the surface chemistry of the sample, will increase the number of analyzable samples for SIMS imaging. The second method covered in Chapter 4 is freeze-etching, the practice of removing excess surface water from a sample through sublimation into the vacuum of the analysis environment. This method was used to cryogenically preserve single cells for ToF-SIMS imaging analysis. By removing the excess water, which condenses onto the sample in vacuo, a uniform surface is produced that is ideal for imaging by static SIMS. I demonstrate that the conditions employed to remove deposited water do not adversely affect cell morphology and do not redistribute molecules in the top most surface layers. In addition, I found water could be controllably re-deposited onto the sample at temperatures below -100 oC in vacuum. The re-deposited water increases the ionization of characteristic fragments of biologically interesting molecules 2-fold without loss of spatial resolution. The utilization of freeze-etch methodology will increase the reliability of cryogenic sample preparations for SIMS analysis by providing greater control of the surface environment. Using these procedures we have obtained high quality images and spectra with both atomic bombardment as well as C60+ cluster ion bombardment. Sample handling is also the topic of Chapter 5. It this chapter, I describe a device which has been designed to prepare frozen, hydrated single cell cultures with a freeze fracture methodology for ToF-SIMS analysis in an ION-TOF (GmbH) TOF-SIMS IV mass spectrometer. The device reproducibly produces frozen hydrated sample surfaces for SIMS analysis. I show that SIMS analysis with the Bi32+ produces high-resolution molecular images of single PC12 cells in an ice matrix. I also show that the combination of ionization enhancements that are provided by both the ice matrix and the cluster ion source facilitates the localization of lipid ions that have not been localized in these cells previously. Namely, two fragments of phosphatidlyethanolamine (m/z 124 and m/z 142) and a large fragment of phosphatidylcholine (m/z 224). The ability to localize and measure these ions will increase the number of question that SIMS imaging can be used to answer. In Chapter 6 ToF-SIMS imaging was used to demonstrate that lipid domain formation in mating single-cell organisms is driven by changes in membrane structure. Studies of lipid bilayers in both living and model systems have revealed that lipid composition is coupled to localized membrane structure. However, it is still not clear if the lipids that compose the membrane actively modify membrane structure or if it is structural changes that cause lipid heterogeneity. I report that time of flight secondary ion mass spectrometry images of mating Tetrahymena thermophila acquired before, during and after mating demonstrate that lipid domain formation, identified as a decrease in the lamellar lipid phosphatidylcholine, does not precede structural changes in the membrane. Rather, domains are formed in response to function during cell-to-cell conjugation. ToF-SIMS imaging has been used to collect information with wide implications in all membrane processes. The work presented here is the continuation of a project aimed at chemically characterizing biological samples with spatially resolved mass spectra, with a particular focus on single cell imaging. Much of the work I have done has centered on understanding the capability of current technology and using this understanding to solve a particular problem. This work is vital to keeping SIMS in the biological realm but the development of new technology is the ultimate future for these experiments by increasing the number of tools that the experimenter has to choose from. In Chapter 7 discuss two ongoing projects that I think will lead to the next break through bringing us closer to realizing the goal of this project: a complete chemical map of a single cell.