Short courses in scanning electron microscopy (SEM) can quickly sharpen practical skills for industrial microscopists. The SEM and the energy-dispersive X-ray spectrometer (EDS) together constitute one of the most powerful and versatile instruments available for solving industrial problems, but interpreting images and spectra is not quite as simple as acquiring them. Applications of SEM span many disciplines, and each application may require knowledge of different aspects of the microscope, and of the industrial problem at hand, to successfully interpret the images and data obtained. Regardless of the problem, whether transistors or trachea cells, the interpretation of SEM images relies upon the microscopist's understanding the fundamentals of image formation as well as the practical aspects of specimen preparation and microscope operation. Many people using SEMs today have not taken any courses beyond the on-site and demo-lab instruction provided by SEM vendors. Equipment manufacturers provide excellent training on how to use the knobs and menus on the SEM to produce useful images and data via the embedded software functions. Since there are many options and setup procedures, these instrument-specific courses are valuable for the novice and expert alike.

Our web submission system, Manuscript Central by ScholarOne, has been in operation since September 1, 2006. The present issue of Microscopy and Microanalysis contains the first paper to appear in print after traversing this system electronically (see the paper by Fuseler et al.). The time elapsed from submission to print publication was under seven months. This is a significant improvement over the old paper-based methods where a manuscript often took more than a year to appear in print.

On September 1, 2006, the Microscopy and Microanalysis electronic submission and review website went live. Our publisher, Cambridge University Press, has teamed with ScholarOne to provide this service. From now on all manuscript submissions to this journal must be made electronically through the following website:

http://mc.manuscriptcentral.com/mam

In 1956 Duncumb and Cosslett developed the first imaging method capable of showing the location of elements in a solid with a spatial resolution of a micrometer. This technique was dubbed “X-ray mapping” probably because a separate image was used to show the presence or absence of each element within the field of view. Since its first demonstration, X-ray mapping has become one of the most popular and useful methods of X-ray microanalysis. It has been widely applied in areas of biology, chemistry, physics, geology, environmental science, and materials science.

This review traces the development of X-ray mapping from its beginning 50 years ago through current analysis procedures that can reveal otherwise obscure elemental distributions and associations. X-ray mapping or compositional imaging of elemental distributions is one of the major capabilities of electron beam microanalysis because it frees the operator from the necessity of making decisions about which image features contain elements of interest. Elements in unexpected locations, or in unexpected association with other elements, may be found easily without operator bias as to where to locate the electron probe for data collection. X-ray mapping in the SEM or EPMA may be applied to bulk specimens at a spatial resolution of about 1 μm. X-ray mapping of thin specimens in the TEM or STEM may be accomplished at a spatial resolution ranging from 2 to 100 nm, depending on specimen thickness and the microscope. Although mapping has traditionally been considered a qualitative technique, recent developments demonstrate the quantitative capabilities of X-ray mapping techniques. Moreover, the long-desired ability to collect and store an entire spectrum at every pixel is now a reality, and methods for mining these data are rapidly being developed.

With this issue, Microscopy and Microanalysis begins its eleventh year of publication. Our journal is getting better year-by-year. In 2004 this journal published more scientific articles than in any previous year. The first biological special issue, on parasites, increased the prominence of the life sciences within these pages. The growing popularity of the journal is also indicated by several letters to the editor about matters arising in certain articles. Such scientific exchanges highlight for our readership the subtleties of interpretation regarding advances in science, instrumentation, technique, and theory.

Quantitative chemical analysis by energy-dispersive X-ray spectrometry (EDS) in the environmental scanning electron microscope (ESEM) is difficult. This analysis is complicated by the spread of the electron beam by chamber gas molecules and the necessity for surface charge neutralization. Without charge neutralization, errors in quantitative analysis can range up to 15–20% relative. It is possible to achieve the error expected of traditional EDS, ±5% relative error, using a newly developed surface charge neutralization scheme for the ESEM. Estimates of accuracy and precision are based on studies of the National Bureau of Standards (now National Institutes for Science and Technology) Standard Reference Material 482, a series of certified copper–gold alloys. The scheme for charge neutralization requires an independent path to ground at or near the surface of the specimen. The current through the ground path must be maintained at zero by adjusting the voltage on the Gaseous Secondary Electron DetectorTM when the sample chamber is at a gas pressure of 1–2 torr. This procedure forms the exact number of chamber gas positive ions to neutralize negative electrical charge on the specimen surface from electron bombardment.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Volume 10 of Microscopy and Microanalysis marks this journal's tenth year. The stated aim of the journal remains to provide a forum for original research papers dealing with new microscopy and microanalysis techniques and their applications. Papers are indexed in several databases including MEDLINE(PubMed) and Chemical Abstracts. Also provided are book reviews and a comprehensive calendar of microscopy events. The journal title is owned by the Microscopy Society of America, and the publisher is Cambridge University Press. The journal now ranks among the top microscopy journals in the world. This achievement is directly attributable to the efforts of its many editors, editorial board members, authors, and reviewers. Particularly notable is the work of my two predecessors, Jean-Paul Revel and Dale Johnson. I thank you all.

Microscopy and Microanalysis has made significant strides forward over the past year, and I would like to comment on two of these. First, the Institute for Scientific Information (ISI) ranked this journal third among the nine microscopy journals it indexes. The ranking was in terms of ISI's Impact Factor, which tracks the number of citations to papers published in the journal. A strong Impact Factor indicates that information in the journal is of interest to other workers in the field. Second, the National Library of Medicine (NLM) has selected Microscopy and Microanalysis to be indexed in MEDLINE (PubMed), beginning with the first issue of 2003. As any biologist will tell you, this listing is essential for the electronic visibility of papers in the fast-moving world of life sciences research. I thank Editorial Board member Dave Piston for his efforts in writing the initial letter of application to the NLM.

Beginning with this issue Microscopy and Microanalysis will be published by the Cambridge University Press in New York. The high-quality production standards established by our former publisher, Springer-Verlag, will be maintained and improved over the coming years. Major changes you may notice are the increased number of pages for scientific articles and the decreased cost of subscriptions for institutional libraries and for members of affiliated societies. An indication of the quality and reputation of the journal is shown by our favorable Impact Factor ranking from the Institute for Scientific Information (ISI). In 1999, ISI ranked Microscopy and Microanalysis the number four microscopy journal in the world. The journal is affiliated with eleven microscopy and microanalysis societies around the world making it truly an international communications vehicle. In fact, Microscopy and Microanalysis has the largest paid circulation of any microscopy journal in the world. On behalf of the Editors and the Editorial Board, I thank the authors, reviewers, advertisers, and readers for supporting this journal during its formative years. I look forward to your continuing support.

Uncoated ceramics are difficult to analyze because specimen charging can reduce the energy of the electron beam at the specimen. This effect may decrease the measured k-ratio to a fraction of its expected value. Thin carbon coatings are the usual solution to this problem. However, the coating procedure takes time, and the same coating thickness also must be applied to the standard. in the environmental SEM (ESEM). surface charge can be mitigated at the higher accelerating voltages normally used for x-ray microanalysis. in the ESEM, electrons are accelerated toward an electrically biased electron detector producing a cascade of electrons and ions from the imaging gas (water vapor) as part of the secondary electron imaging process. Positive ions drift toward the specimen and neutralize negative surface charge; however, the degree of neutralization is a function of a number of operating variables.

This paper presents the results of studies concerning the accuracy and precision of x-ray microanalysis (EDS) in the environmental scanning electron microscope (ESEM). The ESEM is distinguished by its use-of gas in the microscope specimen chamber for imaging and for charge neutralization. Previous work on EDS-ESEM has concentrated either on qualitative x-ray microanalysis or on correction methods to the enlarged x-ray spatial resolution due to the electron skirt. Recent work shows that quantitative analysis is possible once charge neutralization can be accomplished in practice.

Accuracy and precision were evaluated in the work presented here using NIST SRM 482 (goldcopper alloys) and NIST SRM K411 (glass beads). The gold-copper alloy wires were prepared by mounting them in epoxy mounts and polishing to a metallurgical finish. The glass spheres were prepared by sprinkling a small amount of the sample onto double-sided carbon tape mounted onto an aluminum SEM stub.

A number of methods have been proposed to correct for the electron beam scattering effects on xray microanalysis in the environmental scanning electron microscope (ESEM). This paper presents an evaluation of two of these methods. The Doehne method is based on the observation that x-ray counts due to the unscattered electron beam increase with decreasing chamber pressure whereas the inverse is true for x-ray counts due to scattered electrons. The x-ray count intercept, at zero pressure, of the regression lines relating x-ray counts to chamber vapor pressure is an estimate of the high-vacuum intensity. The Gauvin method is based on the relationship between x-ray counts and the fraction of the electron beam that is unscattered, fp.The fraction of the unscattered beam is calculated using an equation derived from scattering theory and uses the accelerating voltage, the gas path length, and the chamber vapor pressure.

Abstract: A novel method for the synthesis of polypeptides using polystyrene/divinylbenzene copolymers as solid supports has drawn the attention of medicinal, pharmaceutical, and agricultural chemists because of its utility in combinatorial chemistry and parallel synthesis. In this method, arrays of solid-phase organic synthesis experiments are conducted simultaneously thereby enabling the preparation of large numbers of novel compounds over a short time period. The analysis of organic compounds attached to polymer supports presents unique challenges to chemists. This study presents some results of the application of energy-dispersive X-ray spectrometry (EDS) in the environmental scanning electron microscope (ESEM) to this problem. EDS in the ESEM has the advantages of minimal sample size, speed, and simplicity because the analyses are performed without special specimen preparation. The progress of a two-step synthetic transformation was followed using EDS-ESEM by the presence of a sulfur peak in the first synthetic step and by a bromine peak in the second step. The synthetic products were also evaluated by infrared spectroscopy and by elemental analysis (ion chromatography). The agreement of the qualitative analysis among all three techniques was good. Analysis by EDS-ESEM not only complements current analytical techniques in solid phase synthesis; it also provides insight into the details of the synthetic transformation.

Analysis of nanosize particles by x-ray emission spectrometry in the analytical electon microscope (AEM) is limited by the level of electron current that can be placed in a 1-2 nm excitation beam and by the consequent electron beam damage. The current in the beam limits the number of x-ray counts generated in the particle, while the beam damage may cause changes in particle chemistry, structure, orientation, and location. The objective of “ultimate AEM analysis” is to make useful measurements right up to the limit where beam damage prohibits analysis.

Elemental analysis of sub-10nm metal particles supported on a ceramic support requires a field-emission source operating at 100-300 kV to generate a significant number of x-ray counts from the area under the beam in a reasonable time [1]. The high current density in the beam of such an instrument can cause damage to the particle or to the underlying support material.