Spring 2016 Syllabus
GEO SCI 545 (LEC 001) – X-ray Analytical Methods
Department of Geosciences, UW-Milwaukee
Dr. Lindsay J. McHenry
This course is designed to train advanced undergraduate students and graduate students in the science and uses of X-ray analytical methods in geological research. This course will provide a background in the physics, chemistry, and mineralogy needed to produce, use, and interpret X-ray Diffraction and X-ray Fluorescence data. It will also provide hands-on training in sample preparation and on modern analytical instruments, and will allow students to pursue individual research projects in their areas of interest.
Prerequisites: Geo Sci 301, Chem 102, OWC-A (English 102 or equivalent placement), jr standing. This course satisfies UWM’s undergraduate OWC-B (Oral and Written Communication-B) GER requirement.
Lecture:
Location: Lapham 262 (lecture), Lapham 336, 377, or 323 (lab)
Time: ~3 hours per week, Tuesday and Thursday, 12:00-12:50.
Lab practical: Group 1 Thursday, 1-1:50;Group 2 ???
Office Hours:
Location: Lapham 324
Time:Tuesday 11-11:50 and by appointment
Contact Info:
Email:
Telephone: 414 229-3951
Course web page: login to D2L at
General plan:
Tuesdays will be lectures, Thursdays will be demonstrations and lab activities. Readings should be completed before the class for which they are assigned.
The reading list is subject to change!
Readings: Selected readings, from copies, D2L, or reserve:
Bish, D.L., Post, J.E., (Eds.) 1989. Modern Powder Diffraction. Reviews in Mineralogy Volume 20. Mineralogical Society of America.
Buhrke, V.E., Jenkins, R., Smith, D.K. (Eds.) 1998. A Practical Guide for the Preparation of Specimens for X-ray Fluorescence and X-ray Diffraction Analysis. Wiley-VCH, New York.
Clearfield, A., Reibenspies, J., Bhuvanesh, N., 2008. Principles and Applications of Powder Diffraction. Blackwell Publishing/Wiley.
Dinnebier, R.E., Billinge, S.J.L., 2008. Powder Diffraction: Theory and Practive. RSC Publishing, Cambridge, UK.
Jenkins, R., 1999. X-ray Fluorescence Spectrometry. Wiley-Interscience, New York.
Jenkins, R., Snyder, R.L., 1996. Introduction to X-Ray Powder Diffractometry. Wiley-Interscience, New York.
Moore, D.M., Reynolds, R.C. Jr., 1997. X-ray Diffraction and the Identification and Analysis of Clay Minerals. Oxford University Press, Oxford.
Obenauf, R.H. et al., (Eds.), 2005. Handbook of Sample Preparation and Handling. Spex SamplePrep, Metuchen, NJ.
Perkins, D., 2011. Mineralogy 3rd Ed. Prentice Hall, New Jersey.
Tertian, R., Claisse, F., 1982. Principles of Quantitative X-ray Fluorescence Analysis. Heyden, London.
Other Required Materials:
Scientific Calculator- you must bring this to every lab session. (An adequate scientific calculator need not have any graphing or programming capabilities, but should have basic arithmetic and trigonometric [e.g., sin, cos, tan] functions. This type of calculator costs as little as $10.)
Ruler with English & metric units- you must bring this to every lab session.
Pencil-you must bring this to every lab session (not a bad idea for lecture either!).
Evaluation
Final course grades will depend on performance in the following areas.
Points Date
UGG
Lab exercises2015
HW and in-class activities105
Quizzes 105
Research project
Reading list and topic5 5February 16
GSA (UG) grant proposal- 1st draft5February 25
GSA (Grad) grant proposal- 1st draft5February 25
Peer review55March 3
Proposal presentation510March 8
Revised GSA (UG) proposal10March 10
Revised GSA (Grad) proposal15March 10
Research paper- 1st draft55April 26
Peer review55May 5
Final research paper1010May 12
Final presentation (UG: 10 min)10May 10 or 12
Final presentation (Grad: 15 min)15May 10 or 12
Lab exercises: most of these will be group efforts since we don’t have13 sets of all of the needed tools! However, all students are required to hand in their own, individual lab reports (with the names of their lab group members) for each.
Quizzes will occur every few weeks and cover the salient points of the most recent lectures. Don’t forget to bring a calculator!
Attendance is required, and will be assessed through the timely completion of lab exercises, in-class activities, and quizzes. Late and unexcused make-up work may be accepted, but with a 10% penalty per class session unless prior arrangements have been made.
Research Project
Each student will select, propose, conduct, and report a research project over the course of the semester making use of the available lab equipment. This can be something related to their own research or using samples provided by the professor (or another professor).
Students must arrange a meeting with the Professor during the 3rdweek of classes to discuss possible research topics and writing skills. A one-paragraph topic statement, plus a list of at least 5 relevant sources, is due on February 18.
The research proposal will be in the format of a Geological Society of America student research grant proposal (~5-6 pages). The proposal presentation will be 5 minutes for undergraduate students ant 10 minutes for grad students.
For the peer review component, each student will review proposal or paper drafts from at least two other students.
The final paper will be in the format of a manuscript submitted to the journal Geology (~8 pages). For undergraduate students, the final presentation will be 10 minutes long. For graduate students, the final presentation will be 15 minutes long.
Broad course goals and objectives
This course is designed such that students will:
• Understand how and why chemical and mineralogical information can be obtained using various X-ray analytical methods.
• Design, propose, conduct, and report an individual analytical research project.
• Gain hands-on experience with both sample preparation and XRD and XRF instrumental methods.
• Judge the quality of geochemical data by calculating errors and counting statistics.
By the end of this course, it is the instructor’s hope that all students will be able to conduct independent, unsupervised analytical research using UWM’s X-ray labs and equipment.
Course outcomes
This course addresses the development of advanced skills in each of the following:
• Critical reading, logical thinking, and the use of argument and evidence (research proposal, research paper).
• The use of appropriate stylistic and disciplinary conventions in writing and speaking (research proposal, research paper, and research presentations).
• Critical analysis of information from primary or secondary sources for some portion of the speaking and writing (research proposal, research paper).
This syllabus is subject to change
WK
/Day
/Date
/Lecture Topic
Assigned readings
1 /Tue
/ Jan 26 / ONLINE LECTURE: The basics: what x-ray analysis can do for you!Thurs
/ Jan 28 /ONLINE LECTURE: A history of X-rays, and x-ray safety
Perkins, 2011, Chapter 12
2 /Tue
/ Feb 2 / X-rays and X-ray diffractionMoore and Reynolds, Chapter 2
Thurs / Feb 4 /
Lab tour and Lab 1: Sample prep for XRD
Bish and Post 1989, Chapter 43 / Tue / Feb 9 /
Diffraction and Bragg’s Law
Moore and Reynolds, Chapter 3 p. 61-80.Thurs / Feb 11 /
Lab 2: The X-ray Diffractometer
Bish and Post 1989, Chapters 2 and 3All / Week /
One-on-one meetings: project ideas!
4 / Tue / Feb 16 /Miller indices and the unit cell
Perkins, 2011, Chapter 11
*** Project topics and reading list due ***Thurs / Feb 18 /
Lab 3: Interpreting XRD patterns
Bertin, 1998, Sections 6.1, 6.25 / Tues / Feb 23 /
Group presentations/discussion: Archaeological uses of XRD. Possible readings: Boszhardt, R.F., Gunderson, J., 2003. X-ray powder diffraction analysis of early and middle woodland red pipes from Wisconsin.
Schreiner, M. et al., 2004. X-rays in art and archaeology: An overview.Thurs / Feb 25 /
Lab 4: Quantitative XRD: Rietveld refinement
Clearfield et al., 2008, Chapter 8*** 1st draft project proposals due ***
6 / Tues / Mar 1 /
Clay mineralogy Bish and Post 1989, Chapter 6.
Thurs / Mar 3 /Lab 5: Clay mineral sample preparation
Moore and Reynolds, 1997, Chapter 6.*** peer reviews due ***
7 / Tue / Mar 8 / *** Project proposal reports (oral) ***
Thurs / Mar 10 /
Lab 5: XRF sampling and sample prep considerations
Buhrke 1998, Chapter 1*** revised proposals due ***
SPRING BREAK
8 / Tue / Mar 22 /Introduction to XRF analysis
Jenkins 1999, Chapter 5
Thurs / Mar 24 / Catch-up (or no lab), depending on our progress9 / Tue / Mar 29 /
Excitation and scattering of X-rays
Tertian and Claisse, 1982, Chapters 2 and 3Thurs / Mar 31 /
Lab 6: Sample preparation: Fused beads
Obenauf et al. 2005, Section 2 Chapters 3 and 4, and Tertian and Claisse 1982, section 18.3All / Week / One-on-one meetings. Project execution (and writing)
10 / Tue / Apr 5 /
Matrix effects, absorption, and enhancement
Jenkins 1999, Chapter 11Thurs / Apr 7 /
Qualitative XRF analysis
Jenkins 1999, Chapter 6Lab 7: XRF operation, data processing
11 / Tue / Apr 12 / Counting statistics, calibration, and data interpretation.Readings TBD
Thurs / Apr 14 / Lab 8: Pressed pellets
12 / Tues / Apr 19 / Group presentations/discussion: other uses of X-rays
Thurs / Apr 21 /
Absorption, mass absorption exercises
13 / Tues / Apr 26 / Energy Dispersive XRFReadings TBD
*** Research paper 1st draft due ***
Thurs / Apr 28 /
Niton handheld XRF demo
Craig, N., et al., 2007. Comparison of XRF and PXRF for analysis of archaeological obsidian from southern Peru. Journal of Archaeological Science 34: 2012-2024.14 / Tues / May 3 / Errors and repeatability
Readings TBD
Thurs / May 5 / Quantitative major and trace element analysis
Future directions in X-ray analysis
Ice et al., 2011. The race to X-ray microbeam and nanobeam science. Science 334: 1234-1239.
*** Peer reviews due ***
15 / Tues / May 10 /*** Final Presentations ***
Thurs / May 1212:30-2:30 /
*** Final presentations ***
*** Final paper due ***Learning Accommodations
I believe it is both important and appropriate to make accommodations that facilitate and improve the learning environment for all students. If you will need accommodations in order to meet any of the requirements of this course, please contact me as soon as possible. We may want to consult the Student Accessibility Center (229-6287; to help assist in devising an appropriate solution.
Accommodations for Religious Observance
Accommodations will be made if you need to miss class and/or a required assignment for a religious observance. Please inform me in advance so that appropriate arrangements can be made.
Teaching Policies
As a student in this course you are responsible to abide by the Department of Geosciences teaching policies and all University established policies. Scholastic dishonesty of any type will not be tolerated. Scholastic dishonesty, a breach of the standards of academic integrity, includes, but is not limited to, cheating, plagiarism, and any act designed to give unfair academic advantage to the student. In this course, the work you hand in for credit must be entirely your own work, except when group work is specifically permitted. Even if you work with others, you are expected to hand in individual assignments written in your own words. You are welcome to discuss any course related problems or issues with me. My goal, and that of the department, is to create a productive learning environment for all students.
More information on University policies regarding course syllabi is available at
Class participation is an important part of the course. You are expected to come prepared to class and to take an active role in class discussions and projects.
Credit-hour policy: This course is designed so that students will spend about 3 hours a week (45 hours total) in class or doing supervised lab activities, about 2 hours a week on course readings and studying (30 hours total), about 2 hours a week on homework (30 hours total), and an average of 3 hours a week on the research project (less time early in the class, more later: 45 hour total). This totals 150 hours, or 50 hours/ credit hour.
This syllabus is subject to change!