In the Classroom
Instrumental Proficiency Program for Undergraduates
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Duane E. Weisshaar,* Gary W. Earl, Milton P. Hanson, Arlen E. Viste, R. Roy Kintner, and Jetty L. Duffy-Matzner Department of Chemistry, Augustana College, Sioux Falls, SD 57197; *
[email protected] Modern chemists rely heavily on instrumental techniques, so education of budding chemists in colleges and universities needs to include hands-on experience with modern instrumentation. A series of programs offered by the National Science Foundation over the last few decades has helped institutions obtain modern instrumentation for this use, and this Journal is filled with examples of experiments utilizing these instruments at all levels of the curriculum. Most of the experiments are “single purpose” in nature, focusing on analysis of a specific sample type or reaction or on one particular facet of the instrument’s capability. A few experiments have focused on the comparison of instruments or techniques (e.g., 1, 2 ) or the use of a single instrument in a broader perspective (e.g., 3, 4 ). These experiments serve well to introduce students to the basics for each instrument. However, in such a program, students use each instrument for two–four hours at a time, work up the data, and move to something else, but seldom have the time on the instrument to gain thorough proficiency. An added consequence, especially in smaller schools, is that the instruments are used intensively for a week or two and then sit idle until the next semester or year. Also at smaller schools care and maintenance of the instruments usually fall on the faculty, tasks that are typically not considered part of the faculty load. To address these and related issues an instrument proficiency program was developed with the following goals in mind: • Provide chemistry majors and other interested students with an opportunity to achieve conceptual and operational competency on the major instruments in the department. • Provide better training for our undergraduate lab assistants so they are able to set up and operate instruments for labs with less instructor interaction, freeing the instructor for other tasks. • Provide on-going care and maintenance for instruments to ensure that they remain ready for use as they are needed. • Provide a means for bringing new instrumentation into the curriculum quickly and easily (development of labs for courses as a proficiency project). • Achieve the above goals without adding unduly to faculty teaching loads.
The program achieves these goals by: (i) a series of one-credithour instrument-proficiency courses, each focusing on the theory and operation of one or two instruments, and (ii) an instrument maintenance and training component for lab assistant assignments.
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Instrument Proficiency Courses A cap on the number of credit hours from a single department that may be counted toward graduation has precluded requiring the proficiency courses for the chemistry major. Thus, these courses were designed to complement standard coverage in traditional courses, rather than a replacement for lab modules or for the instrumental analysis course. Traditional courses provide an introduction and a breadth of experience. The proficiency courses offer an opportunity for added depth of experience: to delve deeper into the theory, more hands-on experience, or introduction to extended techniques, for example, headspace GC, KBr pellets for IR, specular reflectance for IR, and so forth.1 Currently six courses focusing on instrumentation typically encountered in the scientific workplace (not just chemistry) are available: (i) an Anasazi EFT-360 FTNMR (60 MHz), (ii) a Nicolet Avatar 360 FTIR, (iii) a Hewlett-Packard GCD GCMS, (iv) an Ocean Optics R2000 Raman, (v) an HPLC (components from several vendors controlled by PeakSimple software), and (vi) an Ocean Optics SP2000 UV– vis coupled with a Buck Scientific VP-210 Flame AA. The courses are designed for self-directed study, relying on resources like the Analytical Chemistry by Open Learning (ACOL) series (5), selected computer-based training (CBT) programs (6) the Internet (the Analytical Sciences Digital Library Web site, ref 7, is an especially rich resource), and other textual resources to present the theoretical background. In the hands-on portion of the course, the student learns operation, care, and maintenance through at least two studentchosen applications focusing on several features of the instrument. These projects may be used for developing labs for other classes. Because students are introduced to the NMR, IR, and GCMS in the second semester of organic chemistry, this course is a corequisite for these instrument proficiency courses. The other proficiency courses have quantitative analysis, typically taken after second-semester organic at this institution, as a corequisite. For student convenience, texts and CBT materials are supplied. Some, like the ACOL series, were purchased by the library, while others, like the CBT materials, were purchased by the department and are available in the department computer lab. Syllabi that spell out the activities expected for a grade of C, B, or A without dictating content for each course are given to the students. This ensures students have clear guidelines for course expectations while providing flexibility to pursue avenues of personal interest and allowing for individual faculty “stamps of expertise” on that instrument. The Supplemental MaterialW includes examples of syllabi that illustrate course content and a bit of the variation introduced when faculty responsibility is rotated.
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In the Classroom
One proficiency course is offered each semester. We are discussing the pros and cons of pairing up the instruments encountered in a course (similar to the AA and UV–vis course) or offering more than one course each semester to provide opportunity for students to complete all the proficiency courses in four semesters. The main concern is staff time. While the self-directed nature of the courses reduces the faculty time commitment for the course, the load is enough that it needs to be accounted for in that faculty member’s load. Recently we experimented with offering the NMR proficiency course during the January interim. In the interim the instructor’s sole responsibility was the proficiency course, which allowed a more traditional approach to teaching, that is, lectures, exams, and more directed labs. The experiment was successful, but it offered no clear advantage over the selfdirected approach, except, perhaps, providing a more in-depth look at the capabilities of the instrument. Instrument Maintenance and Training as Part of a Lab Assistant Assignment To relieve some of the instrument-care load from faculty, we have added aspects of this to lab assistant assignments (about one hour per week for major instruments and a half hour per week for other instruments). Lab assistants, typically chemistry majors, who have completed second-semester organic or quantitative analysis (assignment prerequisites mirror those for the proficiency courses) are assigned supervisory duties for a major instrument. This assignment entails: • In cooperation with the supervising instructor, learning how to set up, operate, and shut down the instrument. • Taking responsibility for the care and routine maintenance of the instrument, notifying the supervisor when supplies or repairs are needed. • In cooperation with the supervising instructor, developing a set of abbreviated operating instructions for the instrument, and working on development of new experiments for incorporation into labs for other courses. • In cooperation with the supervisor, organizing and conducting a training session for other assistants that includes: (i) instrument start up, (ii) operation, (iii) shut down, and (iv) specific precautions for safe operation. The first three include hands-on experience for all participants.
Assistants who do not have a “major” instrument assignment are assigned supervisory duties for other instruments in the department such as pH meters, gravitometer, refractometer, polarimeter, electronic balances, and so forth. This assignment entails: • In cooperation with the supervising instructor, learning how to operate and calibrate the instrument. • In cooperation with the supervising instructor, developing or updating a set of abbreviated operating instructions for the instruments, as necessary.
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• In cooperation with the supervisor, organizing and conducting several training sessions for other assistants. Training includes: (i) instrument set up, (ii) operation, (iii) calibration and (iv) storage, and (v) specific precautions for safe operation. The first four include hands-on experience for all participants.
At the end of each semester these assistants turn in: (i) a computer file of the most recent version of the abbreviated operating directions (if modified or newly developed), (ii) computer file of a progress report or final procedure of any labs being developed, (iii) a list of the students who participated in the training session, and (iv) a computer file of the training session outline that clearly shows how each required aspect was covered. When the program functions as envisioned, a faculty member can simply say to an assistant in lab “Today students will be using … , you are in charge.”, can trust that the instrument is ready to use, and that the assistant will be able to start up the instrument, lead the students through the use of the instrument, and put it “to bed” at the end of the period. Our Experiences The proficiency courses have worked well. The chosen texts, Internet materials, and CBT materials provide the background and theory in a manner that students can readily grasp. Students who have completed these courses achieve a level of proficiency that enables them to use the instruments in other courses or in research without direct supervision. Student perception of the proficiency courses is that they require a lot of work for one credit hour. As a result enrollments have tapered off over time. Initial offerings had enrollments of 6–9 students, but in recent offerings enrollments of 2–3 students are more typical. Most students complete one proficiency course before graduation, but few students take more than one course. Courses focusing on the spectroscopy instruments encountered in organic tend to have higher enrollments than courses on the other instruments not encountered much in the lower-level courses. An interim offering may be a way to increase the number of proficiency courses offered each year, but it did not realize increased enrollments (three students). Some thought has been given to reducing the content of proficiency courses to make them more appealing. If we combine two instruments into one course, content reduction will probably be necessary to keep time expectations reasonable. However, we are reluctant to reduce content with single instrument courses because students will miss the opportunity to learn the more specialized techniques associated with that instrument. Low enrollments seem to indicate that students are skipping an opportunity that could “set them apart from the crowd” after graduation. However, in the last five years there has been an increase in the number of students involved in research where students have gained proficiency on many of the instruments there rather than taking the proficiency courses. We believe there are still a number of students who are taking the short-sighted “I don’t need it” approach and
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skipping the opportunity. In an effort to address this, we have decided to launch an “advertising campaign” to help students realize the importance and uses for each instrument in the chemistry field and the value that instrument proficiency provides for career development. We hope that having a better picture of the value the courses have to offer, students will be more inclined to take them. “Seeing the need” can have an impact. This last January a student returned from an internship in a forensic lab and immediately signed up for the GCMS course because he now saw the need. The instrument supervision aspect of a lab assistant assignment has had “mixed reviews.” The biggest problem is that the assistants have tended to neglect this aspect of their assignment unless faculty “ride herd” on them, which defeats the original purpose of the assignment. The importance of the instrument assignment for the department and for the career development for the assistant will be included in the “advertising campaign” in hopes that students will see instrument supervision assignments as a career development activity and thus worth the time and effort invested. We have also added some “teeth” to the job assignment by requiring participation in a significant fraction of the instrument training sessions as a requirement for reappointment as a chemistry lab assistant in the following year. We have also considered that perhaps we are expecting too much initiative from our assistants. To test this, one of us is making an effort to develop the training exercise and abbreviated operations manual for a couple of the instruments. The assistant’s job will then be to learn, maintain, and train. The hope is that once these tasks are organized by a faculty member, the assistants will carry it on with a minimum of input from the faculty. It is too early to tell whether this will bear fruit. Conclusion In the ten years we have been using this proficiency program, we find that the proficiency courses are working well and meeting their goals. We hope to encourage more students to take advantage of the opportunity to gain proficiency on these instruments. The assistant supervision part of the program has had a positive impact on routine maintenance and incorporation of instruments in the lab, but has not reached its full potential. The challenge that remains is to increase student participation in both facets of the program. With careful scheduling it seems that the proficiencycourse model would work at almost any size institution. Two groups of two or three students each scheduled for one fourhour block each week could easily time-share an instrument. With two such blocks each day, enrollments of some 40–60 students could be accommodated in each proficiency course. The lab assistant program, while providing desirable experiences for undergraduates, was devised primarily to provide faculty relief from instrument supervision using the
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assistants we have. We envision that larger institutions using graduate students for lab assistants would adapt this model to fit that group, rather than trying to include undergraduates in this aspect. Acknowledgments This instrument proficiency program was developed as part of NSF-ILI grant 9350660 that also provided funds for the purchase of the HP GCD. W
Supplemental Material
Examples of the course syllabi for the six proficiency courses are available in this issue of JCE Online. Note 1. At this institution the instrumental course has a flexible lab that encourages students to emphasize instruments they have not encountered in other courses, including electrochemistry and computer data acquisition, which are not covered in current proficiency courses.
Literature Cited 1. McClain, B. L.; Clark, S. M.; Gabriel, R. L.; Ben-Amotz, D. J. Chem. Educ. 2000, 77, 654–660. 2. Choi, S.; Larrabee, J. A. J. Chem. Educ. 1989, 66, 864–865. 3. Davis, D. S.; Moore, D. E. J. Chem. Educ. 1999, 76, 1617– 1618. 4. Callahan, R.; Kobilinsky, L.; Rothchild, R. J. Chem. Educ. 1999, 76, 1332–1333. 5. Analytical Chemistry by Open Learning (ACOL) series, John Wiley & Sons (New York). Each volume focuses on a single technique. 6. Computer-based training modules: (a) GCD System Tutorial, Version A.01.00, Hewlett-Packard, 1995. (b) MS Fundamentals Computer Based Training, Version A.00.03, HewlettPackard, 1993. (c) Interactive AAS, Version 4.0a and Interactive HPLC, Version 4.0a, Cognitive Solutions LTD, Glasgow, United Kingdom, 1997. (d) Analytical Chemistry by Open Learning (Seven Computer-based training programs in analytical techniques), ACOL Office, University of Greenwich; London, England; Open Learning Agency, Burnaby, B.C., Canada, 1992 (DOS). (e) HPLC for Windows, Advanced Chemistry Collection, Special Issue 28, 2nd ed., JCE Software, 2001. (f ) Introduction to Spectroscopy: IR, NMR, CMR, Mass Version 2.0, 1993, by Fred W. Clough, Trinity Software, Ft. Pierce, FL. (DOS-based program that also runs under Windows.) 7. Digital Library for the Analytical Sciences. http:// www.asdlib.org, one of several digital library collections funded by the NSF DUE NSDL program (accessed Mar 2005).
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