GEOL-4700/ Electron Microprobe Analysis. Spring Schedule: 4 days, TBD (contact Julien) Location: BESC 125

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1 GEOL-4700/ Spring 2018 Schedule: 4 days, TBD (contact Julien) Location: BESC 125 The class consists of a total of 4 days, ideally consecutive, including a minimum of 3 days of hands-on work with the instrument. The class can be spread over a couple of weeks, and/or in 8 half-day sessions if necessary. Students signing up for this class must contact Julien to setup a schedule as soon as they are registered. Due to lab space limitations, each class will be limited to 5 participants, and will be repeated depending on the demand until the end of March INSTRUCTOR Dr. Julien M. Allaz Office Hours: TBD julien.allaz@colorado.edu Office: BESC, 222D Lab: BESC, 125A URL: PowerPoint presentations and other course materials will be provided to each student on the first day of class. COURSE DESCRIPTION This course aims to be a complete overview of analytical theory involving electron and X-ray interactions with solid materials, and to provide an in-depth understanding of the scanning electron microscope for micro- and nano-scale imagery (secondary and back-scattered electrons, cathodoluminescence), qualitative analysis by energy dispersive X-ray spectroscopy, and quantitative analysis using an electron microprobe for micro-scale and non-destructive quantitative analysis by wavelength X-ray dispersive spectrometry. The class will focus on practice, with some essential theory. At the end of the class, the student should be able to prepare the instrument for their own analysis, acquire precise and accurate data, and treat (and interpret) the acquired data. Evaluation of students will be based on theory and ability to operate the instrument. FORMAT OF EVALUATION (final exam) A single 1-hour final exam will be held on the last day of the student s 4-day schedule, and will consist primarily of practice on the instrument. Each student will be individually asked to operate the instrument and to answer a series of short answer questions. PERSONAL notes and material provided by the instructor during the class are allowed for reference during the final exam. Personal computers are NOT allowed during the final exam. Version /13/2018 Page 1 of 6

2 MAKE-UP EXAMS Due to time constraints and the use of the electron microprobe laboratory by other researchers, it is imperative that the student attends the final exam day as defined at the beginning of the class. In case of emergency, a make-up exam can be arranged, but should not affect the analytical work that researchers need to perform on the instrument. TEXTBOOKS The first reference is strongly recommended, especially if you intend to use a scanning electron microscope or electron microprobe for your research. Thanks to a special agreement between Springer Edition and CU, this e-book is free when you are on campus or connected by VPN to CU Boulder. The other references are useful for additional information. Prices are purely estimates and not guaranteed; some books might be purchased on the web as used for much cheaper. SEM and EMPA (1) SEM and EMPA Author(s) Year Title Editor / ISBN Price J. Goldstein, D.E Scanning Electron Springer Newbury, D.C. Joy, Microscopy and X-ray ISBN C.E. Lyman, P. Echlin, Microanalysis (3 rd ed.) E. Lifshin, L. Sawyer, J.R. Michael S.J.B. Reed (short version of the following textbook) EMPA S.J.B. Reed 1993 (2011) 2005 Electron Microprobe Analysis and Scanning Electron Microscopy in Geology (2 nd ed.) Electron Microprobe Analysis (2 nd ed.) Cambridge Univ. Press ISBN Cambridge Univ. Press ISBN (1) Free e-book (CU campus agreement): Free e-book (on CU campus) $70 (hardcover) $17 (ebook) $105 (hardcover) $40 (paperback) $53 (print) TEACHING PHILOSOPHY Group discussion and collaboration is strongly encouraged throughout the class, as are questions directed to the instructor. The study of electron microscopy and X-rays / photons can be complex, and asking questions to the instructor as well as your classmates is absolutely necessary to complete the course successfully. Nevertheless, it is absolutely unacceptable to turn in any work that is not your own. This course consists of dual play between theory and practice. The theory will cover the function of the instrument, and all necessary information needed for data treatment (and to some extent, interpretation as well). It is being partly taught using a spiral learning technique such that a few important topics are covered multiple times during the course with each additional exposure focusing on greater detail. Keep all your work in class organized, as these materials will be your most critical study aids throughout the class, during the final exam, and for the next time you will be using a scanning electron microscope or an electron microprobe. It is highly recommended that you purchase a notebook dedicated to your work on the instrument. This will become your lab book, where you will later record all the analysis you perform on the instrument. You can use your own notes for reference during the final exam. Be on time! As we are using laboratory equipment that is also being used by other researchers, it is very hard, if not impossible, to reschedule a time if you miss a class day; if this happens, advise the instructor immediately (by or in person). The use of cell phones in class, along with web Version /13/2018 Page 2 of 6

3 navigation unrelated to the class is not acceptable (including, but not limited to Facebook, Twitter, Instagram, Reddit, Snapchat ). If it is an emergency, step out of the room to avoid class disturbance. Otherwise, leave your cellphone in your bag and in silent mode. ACCOMMODATIONS FOR DISABILITIES If you qualify for accommodations because of a disability, please submit your accommodation letter from Disability Services to your faculty member in a timely manner so that your needs can be addressed. Disability Services determines accommodations based on documented disabilities in the academic environment. Information on requesting accommodations is located on the Disability Services website ( Contact Disability Services at or dsinfo@colorado.edu for further assistance. If you have a temporary medical condition or injury, see Temporary Medical Conditions ( the Students tab on the Disability Services website and discuss your needs with your professor. RELIGIOUS HOLIDAYS AND OBSERVANCES Campus policy regarding religious observances requires that faculty make every effort to deal reasonably and fairly with all students who, because of religious obligations, have conflicts with scheduled exams, assignments or required attendance. See the campus policy regarding religious observances ( for full details. CLASSROOM BEHAVIOR Students and faculty each have responsibility for maintaining an appropriate learning environment. Those who fail to adhere to such behavioral standards may be subject to discipline. Professional courtesy and sensitivity are especially important with respect to individuals and topics dealing with race, color, national origin, sex, pregnancy, age, disability, creed, religion, sexual orientation, gender identity, gender expression, veteran status, political affiliation or political philosophy. Class rosters are provided to the instructor with the student's legal name. I will gladly honor your request to address you by an alternate name or gender pronoun. Please advise me of this preference early in the semester so that I may make appropriate changes to my records. For more information, see the policies on classroom behavior ( and the Student Code of Conduct ( SEXUAL MISCONDUCT, DISCRIMINATION, HARASSMENT AND/OR RELATED RETALIATION The University of Colorado Boulder (CU Boulder) is committed to maintaining a positive learning, working, and living environment. CU Boulder will not tolerate acts of sexual misconduct, discrimination, harassment or related retaliation against or by any employee or student. CU s Sexual Misconduct Policy prohibits sexual assault, sexual exploitation, sexual harassment, intimate partner abuse (dating or domestic violence), stalking or related retaliation. CU Boulder s Discrimination and Harassment Policy prohibits discrimination, harassment or related retaliation based on race, color, national origin, sex, pregnancy, age, disability, creed, religion, sexual orientation, gender identity, gender expression, veteran Version /13/2018 Page 3 of 6

4 status, political affiliation or political philosophy. Individuals who believe they have been subject to misconduct under either policy should contact the Office of Institutional Equity and Compliance (OIEC) at Information about the OIEC, the above referenced policies, and the campus resources available to assist individuals regarding sexual misconduct, discrimination, harassment or related retaliation can be found at the OIEC website ( HONOR CODE All students enrolled in a University of Colorado Boulder course are responsible for knowing and adhering to the academic integrity policy ( Violations of the policy may include: plagiarism, cheating, fabrication, lying, bribery, threat, unauthorized access to academic materials, clicker fraud, resubmission, and aiding academic dishonesty. All incidents of academic misconduct will be reported to the Honor Code Council (honor@colorado.edu; ). Students who are found responsible for violating the academic integrity policy will be subject to nonacademic sanctions from the Honor Code Council as well as academic sanctions from the faculty member. Additional information regarding the academic integrity policy can be found at the Honor Code Office website ( Version /13/2018 Page 4 of 6

5 Abbreviations for (micro-)analytical techniques In bold = techniques discussed during this class AES AFM APT (APM) ARPES BSE CFM EBSD EDS EELS EMPA (EPMA) ESCA FE FIB FIM FTIR IRRAS LA-ICP-MS LEED LEIS LEXES MFM PEEM PIXE Auger Electron Spectroscopy Atomic Force Microscopy Atom Probe Tomography (Atom Probe Microscopy) Angle-Resolved PhotoEmission Spectroscopy Back-Scattered Electron ConFocal Microscopy Electron BackScatter Diffraction Energy Dispersive (X-ray) Spectrometry Electron Energy Loss Spectroscopy Electron MicroProbe Analysis (Electron Probe MicroAnalyzer) Electron Spectroscopy for Chemical Analysis Field Emission (gun) Focused Ion Beam Field Ion Microscope Fourier Transform InfraRed spectroscopy InfraRed Reflection-Absorption Spectroscopy Laser Ablation Inductively Coupled Plasma Mass Spectrometry Low-Energy Electron Diffraction Low-Energy Ion Scattering Low Energy (electron induced) X-ray Emission Spectroscopy Magnetic Force Microscopy PhotoEmission Electron Microscopy Proton Induced X-ray Emission (µ-) Raman (micro) Raman (inelastic) scattering spectroscopy SE Secondary Electron SEM Scanning Electron Microscope SHRIMP (nano) SIMS SPM STEM STM TEM UV-VIS WDS (NE)XAFS XANES XPS Sensitive High Resolution Ion Microprobe Secondary Ion Mass Spectrometry Scanning Probe Microscopies Scanning Transmission Electron Microscopy Scanning Tunneling Microscopy Transmission Electron Microscopy UltraViolet-visible spectroscopy Wavelength Dispersive (X-ray) Spectrometry (Near Edge) X-ray Absorption Fine Structure X-ray Absorption Near Edge Structure X-ray Photoelectron Spectroscopy (µ-) XRD (micro) X-Ray Diffraction (µ-) XRF (micro) X-Ray Fluorescence Version /13/2018 Page 5 of 6

6 SCHEDULE The following schedule is subject to change over the duration of the course. Part 1 and 2 will be covered in 1 to 1.5 days, the rest of the class will concentrate on Part 3. Bring your sample! Part 1 Hardware and basic principles for electron microscopy 1. Sample preparation Sample mounts, epoxy, polishing, coating 2. Generalities on the hardware Vacuum system, gauge, electron column, detectors, computers 3. Electron optics emitters Electron sources: W, LaB 6 (CeB 6 ), field-emission (cold, thermal, Schottky) Electron gun, gun bias, beam saturation 4. Electron optics lenses Electron deflection by electromagnetism: condenser & objective lenses Beam aperture, beam current regulation, beam size Working distance, depth of field, aberrations and corrections Part 2 Specimen interactions: electron scattering & signal generation 5. Beam - Specimen Interactions Back-scattered electron (BSE), secondary electron (SE) X-ray continuum (Bremsstrahlung), characteristic X-ray, binding energies Energy (EDS) versus wavelength (WDS) measurement Analytical and spatial resolution Other interactions: electron back-scattered diffraction, Auger process, cathodoluminescence, etc. 6. Signal detection Electron detectors: density contrast (BSE) versus surface / topography (SE / TOPO) imaging Scanning and image formation, area & resolution, depth of field EDS detectors: silicon-lithium detector Si(Li) versus silicon drift detectors SDD Wavelength Dispersive Spectrometer (WDS), monochromators, geometry (Bragg s law) X-ray detector for WDS, Pulse Height Analysis (PHA) Part 3 Qualitative and quantitative analyses 7. Quantitative Analysis Electron interaction, analysis of characteristic X-ray From counts to weight-percent: the matrix correction Simple examples of applications 8. Statistics Precision, accuracy, sensitivity (detection limit), source of error, spatial resolution Short-term (random versus systematic) / long-term errors, counting statistic Challenge of trace element analysis: background, interferences, beam damage Peak shift and other potential analytical problems 9. Applications (at least one full day!) Using the right program, with the right options, and the right parameters to obtain what you need This part of the class will be adjusted to the class interest If a student has a suitable sample to be investigated, and if the project is deemed feasible in the allocated time, a student s sample might be loaded for a real-case scenario work. Version /13/2018 Page 6 of 6