Fall 2009 CONFCHEM	Excellence in Education with CCLI: Notes from Recent Awardees An on-line conference, September and October 2009
	Abstracts	Papers	Instructions	Discussion Archive

 

"A Tale of Two Universities: Collaborative Proposals in the CCLI Program"

Gary Trammell (trammell.gary@uis.edu),  Keenan Dungey

University of Illinois Springfield, Department of Chemistry, One University Plaza, Springfield, IL 62703;

Eric J. Voss

Department of Chemistry, Southern Illinois University Edwardsville, Edwardsville, IL 62026-1652.

Abstract:

The University of Illinois Springfield (UIS) and Southern Illinois University Edwardsville (SIUE) have collaborated on two successful NSF CCLI/A&I grants.  These grants enabled our institutions to purchase advanced instrumentation for each school and incorporate them across the undergraduate chemistry curriculum.  One grant funded powder X-ray diffractometers, and the second provided scanning probe microscopes.  Each institution has one of “twin” instruments to help in sharing experiments, protocols and to aid in troubleshooting.  This partnership pairs a small public liberal arts institution (UIS) in which faculty teach all lab sections with a medium-sized public institution (SIUE) with a large undergraduate chemistry enrollment with graduate teaching assistants in laboratories.  Cooperation was enhanced through joint training and monthly meetings held at alternate institutions, along with frequent e-mail exchanges.  This paper will discuss the advantages of cooperation between these two types of institutions for developing and assessing lab activities.  Besides collaboration between institutions, these projects involve cooperation among faculty teaching across the curriculum since these instruments are used in introductory, general, organic, analytical, physical, inorganic chemistry and in undergraduate research projects.

Introduction:

In developing our projects, collaboration was the dominant theme.  We developed a collaboration to share the use of advanced instrumentation between two institutions of different sizes and missions and among chemical disciplines. We saw adding advanced instrumentation as a means for rethinking and updating our curriculum to better engage our students with the goal of increasing enthusiasm for science in our students.  At the start of each project only a few faculty members were familiar with the technique. These faculty members helped train other members of the department in different chemical disciplines to make the program integrated throughout the curriculum.

As a result of our collaboration we have been able to share laboratory experiments, assessment tools, and research ideas between institutions.  We have also been able to look at the curriculum at each institution and develop strategies for introducing instrumentation in general chemistry and expanding their use through the curriculum. Since we began this collaboration in 2002, a dozen faculty members and thousands of students have had direct experience with the advanced techniques of powder X-ray diffraction and scanning probe microscopy. 

Starting a Collaborative Proposal

When UIS hired a new inorganic chemist with a strong interest in materials science, we knew that a powder X-ray diffractometer was an important tool for his research.  The price of the instrument far exceeded our university equipment budget.  For several years we were able to use an instrument at the University of Illinois Urbana-Champaign.  The time and cost of using this instrument made development of research slow and made it difficult for our undergraduates to have experience with this technique.  When we decided to pursue a NSF-CCLI grant to purchase an instrument, our inorganic chemist (Keenan Dungey) knew that Eric Voss of SIUE was also interested in materials science.  He contacted Eric looking for a letter of interest in sharing instrument time.  Eric responded right away that he was planning to write his own proposal, but he’d heard of the Collaborative Proposal program at NSF.  We looked into the guidelines and decided that a joint proposal would be stronger than separate proposals from institutions 80 miles apart.  In addition, we found additional mutual interests, including pre-existing collaborations with the UW-MRSEC group (http://mrsec.wisc.edu/Edetc/).  Gary Trammell, an organic chemist at UIS, had experience in teaching materials science to high school teachers through workshops at UIS and the Institute for Chemical Education.  We realized that using the instrument for one or two faculty members’ research was not an effective use of an expensive resource and were interested in integrating powder X-ray diffraction throughout the curriculum, much like IR and NMR spectroscopy have become integral in undergraduate training.

Our two institutions involved in the collaboration have different mandates and organizations.  UIS is a public liberal arts university and is the smallest member of a large three-campus system.  UIS offers only a BS (ACS approved) degree in chemistry.  The institution has an enrollment of approximately 2,900 undergraduate and 2,000 graduate students.  The six faculty members in chemistry teach their own labs without aid from teaching assistants.  Each semester we teach about 5 sections of general chemistry and two sections of organic.  SIUE is a public university, also part of a multi-campus system, with an enrollment of approximately 13,600 students.  The Chemistry Department at SIUE offers BS and MS degrees and has about eighteen faculty members.  Introductory labs at SIUE are taught by graduate teaching assistants. 

Structure of a CCLI Collaborative Proposal

In a CCLI Collaborative Proposal, two (or more) institutions apply jointly through FastLane.  Each institution has a PI and a budget, but they share the same Project Summary and Project Description.  The combined budget requested from NSF for both institutions, including indirect charges, must be less than the maximum allowed.  The maximum award for collaborative proposals depends on the type of project (http://www.nsf.gov/pubs/2009/nsf09529/nsf09529.html).

Writing the proposal required many e-mails until both PIs were agreed on the Project Summary and Description.  We also had to coordinate our budgets, and we were able to realize some cost savings by sharing training and assessment expenses.  Each PI communicated with the grants office at his home institution to complete the submission on FastLane.  Ultimately, one institution presses the Submit button, and that PI calls the other to confirm and they both heave a sigh of relief.

Tips on preparing a CCLI Collaborative Proposal:

• Talk with the Program Officer.  This is what helped us determine to try a Collaborative Proposal rather than compete with each other.
• Find a collaborator.  Do you know someone at a nearby institution with similar interests? 
• Discuss what synergies the collaboration will realize.  With our two different types of institutions, there was an advantage in being able to share results.
• Find a committed team of faculty.  Get them on board as co-PIs with a budget line and a biographical sketch.  This demonstrates to the reviewers that you’re serious about the amount of involvement of the other faculty, more than just a paragraph stating how they might use the instrument.
• Get institutional support.  While no match is required by NSF, and the amount of money the institution commits doesn’t sway the reviewers, the type of support the institution can provide demonstrates the likelihood of the project succeeding.  Our institutions were able to provide consumables, hire student workers and defray travel expenses related to the grant.
• Consider the scope of the project and plan the schedule accordingly.  With our instrumentation, we knew there would be a delay involved in the purchasing and installation and training.  We also wanted to be able to try a new experiment at one institution and then share the results with the other institution, so we needed at least 2 years for a full cycle of the project.

The First Proposal:  Incorporating Powder X-ray Diffraction Throughout the Undergraduate Chemistry Curriculum 

Working together on the NSF-CCLI proposals brought together a critical mass of faculty interested in bringing new experiments and technology into the undergraduate curriculum. Each faculty member involved had something to contribute and by sharing resources we could develop new laboratory activities much easier than if we were doing this individually.  All of the co-PIs met each month (at alternating institutions) in order to plan experiments, report on progress, share ideas, exchange handouts, and update assessments.  We also received joint training on the instrument.  While meeting face-to-face required extra traveling time (UIS and SIUE are about 90 minutes apart), everyone involved felt that the time was well spent as the meetings were efficient and effective.    

Initially we developed objectives for our project and student learning objectives.  With these in mind we were able to see ways to use the instrument in different courses to build on our students’ previous experience. Table 1 summarizes the X-ray diffraction and related experiments carried out at our institutions.

Table 1. Powder X-ray Diffraction Experiments at SIUE and UIS

* A general education course for non-majors.

In the general chemistry lab students are introduced to powder X-ray diffraction in a unit on the structure of the solid state by (1) analyzing physical6 and computer models^{16, 17} of crystal structures (Figure 1), (2) exploring the Institute for Chemical Education (ICE) optical transforms¹⁸ as 2-D analogs of X-ray crystallography and (3) conducting experiments in which they prepare and analyze solid materials using the power X-ray diffractometer.  Each of our powder X-ray diffractometers have a 6 sample changer so it was easy for small groups of students to load their sample and get to see the instrument and identify its components. 

UIS and SIUE shared development of the optical transform activity which introduces Bragg’s law.  Some of the labs used at each institution were different due to interests of the faculty and the different sizes of undergraduate populations.

Figure 1. Students at UIS Exploring Solid State Model Kit (from ICE)

In general chemistry at SIUE, the phosphor Y₂O₃:Eu Phosphor^1,2 is prepared and analyzed before and after heating.   Students prepare aqueous solutions of the reactants in a beaker that is placed in a muffle furnace at 500 °C.  A dramatic reaction explosively produces a foamy white powder that glows red under UV light (Figure 2).  Heat treatment of the nanoparticles overnight at 850 °C results in a powder that fluoresces more brightly, and shows sharper peaks in the powder X‑ray pattern as a result of larger crystallite size.

Figure 2.  Powder X-ray diffraction pattern of Y2O3:Eu3+ before (top powder pattern) and after (bottom trace) heat treatment.

At UIS students perform a solid phase titration of the solid acid zirconium phosphate, Zr(HPO₄)₂_H₂O⁷.   This compound has a lamellar structure, with acidic protons available at the interlayer region of the crystal. These protons can react with aqueous or gaseous bases, such as sodium hydroxide or alkyl amines. Upon reaction, the structure of the zirconium phosphate layers remains unchanged, while the interlayer distance increases to accommodate the guest ion or molecule.  This greatly simplifies the analysis of the powder X-ray diffraction data, as the students calculate only one dimension of the unit cell (Figure 3).

Figure 3  Six-sample changer of X-ray diffractometer.  Powder patterns of  different stages of the titration and the “Oreo cookie” analogy for the change in interlayer distance.

X-ray diffraction is usually covered in the curriculum in advanced inorganic chemistry courses, but to meet our goal of using the instrument throughout the curriculum, we sought ways to use this powerful technique in organic chemistry.  At UIS we developed two labs in which students synthesize a solid product and characterize it by power X-ray diffraction.  In the first semester of organic chemistry a lab was designed to show the application of organic chemistry to new developments in materials science through organic LEDs.  Students prepared the fluorescent complex tris(8‑hydroxyquinoline)aluminum(III), Al^IIIq₃, ⁸ and characterized it by IR and powder X-ray diffraction.  In a companion experiments students constructed the organic LED described in the MRSEC website¹⁹.  Students experienced some difficulty in preparing the organic LED.  The synthesis of Al^IIIq₃ was unproblematic and gave a characteristic diffraction pattern.  Students identified their product by its fluorescence and by fingerprinting their X-ray powder pattern to a reference pattern from the literature.  The structure of the products gives students an introduction into types of isomers not usually encountered in organic chemistry.

Since the student population in organic chemistry at UIS consists of a majority of biology majors a diffraction experiment was developed to investigate urea inclusion compounds as an example of host-guest recognition.  This topic tied in with the lecture and has relevance to biology.  Each student was given a small organic molecule, usually an alcohol or carboxylic acid, and was asked to prepare a solid product using a general procedure.  The solid was analyzed by powder X-ray diffractometry and the pattern compared with the starting material, urea.  If the compound formed an inclusion complex with urea, the size and shape of the crystal changed and students obtained a different pattern.  If the molecule did not complex with urea, the product obtained gave an identical pattern to the urea standard.  A class set of data was prepared and students made conclusions about the size and spatial requirements for complexation.  While students were waiting for instrument time, they did an activity modified from the ICE DNA Optical Diffraction module¹¹.  Students used 2-D optical diffractions to see how Franklin, Crick and Watson determined the structure of B-DNA. 

In advanced inorganic labs, students at both UIS and SIUE prepared the 1,2,3 superconductor^{14, 15} and analyzed its power pattern before and after annealing (Figure 4).

Figure 4.  X-ray powder patterns of  the 1,2,3-Superconductor mixture before (left) and after (right) annealing

The Second Proposal : Incorporating Scanning Probe Microscopy across the Curriculum

We were very excited with the results of collaboration on the powder X-ray diffraction project and elected to pursue a second collaborative CCLI grant to incorporate scanning probe microscopy across the curriculum  The student activities were selected to give students some experience in general chemistry and expand use of the instrument as students progress through the chemistry curriculum.

Table 2.  Scanning Probe Microscopy Experiments at SIUE and UIS

* A general education course for non-majors.

We introduce our students to SPM with a refrigerator magnet (Fig. 5).  When the strip is removed from the side of the magnet, the student now has a working analogy of SPM (from UW-MRSEC website).  They are asked to scan the probe across the surface to map the surface properties.  Students are further prompted to think about how the size of their probe might affect their results, as well as to consider what other interactions (besides magnetic) could be used to image a surface.

Figure 5.  The Refrigerator Magnet analogy of SPM [http://mrsec.wisc.edu/Edetc/supplies/ActivityGuides/Refrig_Magnet_Guide_2005.pdf].

The most common teaching application of SPM is the scanning tunneling microscope (STM) imaging of the surface of highly oriented pyrolitic graphite (HOPG).  Since we wanted students to move beyond the “I saw atoms” understanding of STM, and we found that the actual scanning of a high quality image is time consuming, we spend most of the lab period in our introductory courses on data analysis. 

The students work in pairs at laptops with the SPM analysis software and are provided with raw images from our instrument.  Using the software, students filter the data and measure the distances between the bumps on the surface.  They then try to relate the image pattern and inter-bump distance to the 3D model of graphite (we provide paper projections and ball and stick models) (Figure 6). 

Figure 6.  SIUE students work with a model of graphite.  Student acquired and filtered STM image of HOPG (4nm x 4nm).

Students gain experience with unit conversions (nanometers and micrometers), and improve 3D visualization skills.  One of the take-home points is that the STM images a lattice rather than individual atoms.

Another experiment we have introduced in our 100-level courses is the dynamic Atomic Force Microscopy (AFM) of nickel nanowires.  We first starting having students synthesize the nickel nanowires as part of our X-ray diffraction grant.  These nanowires are prepared by electrochemical deposition of nickel into an alumina membrane, which is then dissolved away to leave rods with a 200 nm diameter and lengths of up to 50 µm (Figure 7).  With dynamic mode, the dry wires can be imaged without the use of adhesive, since the tip of the AFM is not dragged across the surface of the sample.  In this experiment, the students are able to image their own samples, and then measure them using the same SPM Analysis software that they were introduced to in the STM of graphite experiment.

Figure 7.  Preparation of Nickel Nanowires^3,4

During the same lab period, students perform a “blackbox” experiment²⁶ to consider issues of resolution and the limits of imaging only the surface of a 3D object. Students insert a straw into an array of holes in a box lid, measuring the height of the straw at each point, then try to determine the object in the box (Figure 8). This “blackbox” image is then directly related to the AFM image they collected. For example, the apparent image of one rod may actually be due to a clump of two or more rods.

Student acquired AFM image of nickel nanowires (54 µm x 54 µm)	Example of “blackbox” activity for students to learn about probing the surface of a 3D object.26
Figure 8.

In one of our advanced labs, students learn to use another aspect of the dynamic AFM image technique.  In addition to obtaining topographical information of the surface, the phase signal of the oscillating probe can be simultaneously measured and a phase contrast image produced.  The phase contrast is due to relative elasticity (or hardness) differences on the surface of the sample. 

Our advanced inorganic students prepare a bicylic alkene monomer and then synthesize a block co-polymer with cyclooctene using a ring-opening metathesis (ROMP) catalyst²⁴.  The resulting polymer is spin-cast onto an AFM sample holder and the students use the instrument to image their own samples.  While there is little height change for the thin polymer film, there are distinct regions in the phase contrast image (Fig. 9).  The students learn that the different monomers produce materials of different hardness.  The students are asked to consider how the properties of the co-polymer might change given changes to the polymerization conditions. 

Figure 9.  Student acquired AFM phase contrast image of a block co-polymer spin-cast onto mica (50 µm x 50 µm).

Assessment:

Assessing student learning of a lab activity is often a challenge.  To help in assessment we were fortunate to collaborate with Dr. Douglas Eder, Emeritus Director of Undergraduate Assessment & Program Review at SIUE.   Each lab activity was assessed for student understanding.  This section describes results of the X-ray project since it is further along.  We are doing similar assessments for the SPM project.

In order to further refine our student learning goals for the proposed helical curricular changes (a chemistry student would re-encounter diffraction concepts in each year of the undergraduate curriculum in ever increasing complexity) we developed a “top ten” list of important aspects to powder X-ray diffraction (Table 3).

Table 3.  PXRD Top Ten

1. Use a powder X-ray diffraction pattern to identify a material (fingerprint)
2. Recognize that X-rays probe submicroscopic dimensions
3. Understand the unit cell concept and relate it to how solids extend in three dimensions
4. Relate space between atoms to angle of diffraction and Bragg’s Law
5. Chemically change a crystal structure
6. Understand how molecules pack in three dimensions
7. Demonstrate that the properties of materials depend upon crystal quality
8. Relate diffraction intensity to electron density
9. Prepare a sample properly in order to minimize errors in powder pattern
10. Determine unit cell type and dimensions from a powder X-ray pattern

In the introductory chemistry courses, students were asked to define diffraction upon completion of the lab and indicate how confident they were of their definition.  In both the majors and non-science majors sections, over 80% were fairly confident in their definitions.  Their definitions reflected concepts 1, 2 and 4 from Table 3.  Organic chemistry (second year science majors) were asked the same question.  Their results were analyzed according to Bloom’s Taxonomy²⁷.  We were reassured to find that students went beyond a memorization of the definition to include words indicating they had an understanding of the technique and its applications. 

Counting Atoms in Unit Cells

An embedded assessment of Top Ten #3 was carried out in second semester general chemistry at UIS.  Students were asked to count atoms in unit cells based upon 2-D projections as a pre-laboratory activity.  As this topic was also covered in the lecture portion of the course, the students were again asked to count atoms in unit cells on a test given after they performed the diffraction experiments.  In Spring 2005, 0% of students could correctly answer the pre-lab question, while 13/18 (72%) of the same students could answer the test question.  Similar results occurred in Spring 2007: only 5/38 (13%) students got the pre-lab question correct, while 35/38 (92%) got the test question correct.  Analysis of incorrect results indicated that student were confusing 2-D unit cells and 3-D unit cells, so the lecture material was modified.

Bragg’s Law

Another embedded assessment of student learning was carried out in CHE 241general chemistry.  In a post-laboratory question, students were asked to calculate the d-spacing for the solid they prepared (Top Ten #4).  In Spring 2005, science majors at UIS were successful in applying Bragg’s Law, with 16/18 getting a correct answer.   SIUE showed similar results.

As a result of our collaboration between institutions and between disciplines, several thousand students at SIUE and 100 students at UIS received hands-on experience with X-ray diffraction during the grant period.  Eleven faculty members were involved in this project.  These laboratories continue to be taught, successfully institutionalizing the technique.

Conclusion:

We have been very pleased with the collaborations developed in these projects.  The stimulation of working with colleagues on a project of interest is a benefit to all faculty.  We have found the following advantages of collaboration.

Advantages of Collaboration

• Larger pool of faculty members with expertise and/or interest in the instrumentation
• Exchange of successful experiments
• Assistance in troubleshooting labs or instrument problems
• Ability to try out labs with different settings and groups of students
• Help in developing assessment strategies
• Larger group of students to evaluate leaning outcomes

Disadvantages of Collaboration

• Extra communicating
• Travel time (UIS and SIUE are about 90 minutes apart)

Lessons Learned:

By participating in these ongoing collaborative projects, we have learned a few lessons.  In both projects, we had hands-on use of fairly complex instruments by large numbers of students.  One key to success was careful scheduling and design of experiments.  For example, we discovered that the hands-on use of the scanning probe microscope for the STM of graphite was not practical due to the long time needed to engage the tip with the sample.  Instead, students were given previously collected data sets on laptops so that ten groups of students could be measuring carbon-carbon distances simultaneously during the laboratory period.  On the other hand, the AFM of nickel nanowires did work well for hands-on use of the scanning probe microscope, and groups of four students could set up the experiment, collect their own data, and analyze it within the laboratory time allowed.  Other keys to success include efficient training of teaching assistants and faculty coordinators, effective communication between project directors and other stakeholders at each institution, and the continuous exchange of materials between SIUE and UIS for testing and development.  Another lesson learned was that students in introductory courses often experience information overload.  When presenting them with a new technique, an instrument that requires complex directions, and the manipulation of data using unfamiliar software, we tried to focus on a "take home message" that was clear and easy to follow.  For example, in the AFM of nickel nanowires experiment, we stressed the fact that this instrument was scanning a sample (wires on a mica surface) with a probe (the cantilever), and that this was what they should focus on, rather than worrying about all of the details of the manipulation of the instrument parameters.

We have found that collaborations extend beyond our respective departments.  One of us (KD) has made presentations to researchers at Southern Illinois School of Medicine (SIU-SM) and to Clinical Laboratory Scientists on the biological applications of SPM.   He is currently collaborating on a research project on the toxicology of nanoparticles with a researcher at SIU-SM.  Faculty at SIUE have introduced applications of X-ray diffraction and SPM to middle school teachers in summer institutes.  Faculty and students from other institutions have brought students to campus to use our instruments for classroom or research projects.

Acknowledgements:

• National Science Foundation
• CCLI A&I Grant 0410642 (SIUE) and 0410607 (UIS)
• CCLI A&I Grant 0633186 (SIUE) and 0633175 (UIS)
• University of Illinois Springfield
• Southern Illinois University Edwardsville
• University of Wisconsin-Madison MRSEC
• Harshavardhan Bapat -UIS
• Wayne Gade - UIS
• Michael J. Shaw -SIUE
• Masangu Shabangi - SIUE
• Eric G. Malina - SIUE
• Susan D. Wiediger - SIUE
• Leah O’Brien - SIUE
• Douglas Eder – SIUE
• Layne Morsch – UIS
• Marc Klingshirn - UIS
• Jeffrey Cornelius -Principia College
• Undergraduate research students – UIS and SIUE

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