As some of us are frantically "dusting off" and "polishing up" our syllabi for courses this spring, I thought it might be interesting/useful to share lists of experiments that you do in your inorganic laboratory course (if you have one). So, tell us a little bit about your course (level, lab pre-requisites, concurrent or separate with lecture) along with your list of experiment titles. It might also be helpful to indicate if any specialized equipment is needed for an experiment other than standard glassware, IR, NMR, UV/Vis.
So here's my list for Introductory Inorganic Chemistry. This is a sophomore/junior level lecture/lab course with a year of general chemistry as a pre-requisite. Nearly all of the students will also either have one semester of O-chem lab under their belt or else have completed the whole course.
- Exp 1: Experimental Simulation of X-ray Diffraction (Lasers, optical transform slides)
- Exp 2: Introduction to Powder Diffraction (X-ray powder diffractometer)
- Exp 3: Layered Perovskite Project. Part I: Solid State Synthesis. Part II. XRD of Layered Perovskites. Part III. Ion Exchange Chemistry: Layered Perovskite Solid Acids. (High temperature furnace, alumina crucibles, X-ray powder diffracometer)
- Exp 4: Sol-Gel Silica: Nanoarchitectures of Being and Nothingness
- Exp 5: Project Werner. Part I. Synthesis of Cobalt Coordination Complexes. Part II. Swapping Ligands – The Nitrite Exchange. Part III. Spectroscopy and Solution Conductivity of Cobalt Complexes (Solution conductivity probe)
- Exp 6: The Metal Matters. Part I. Synthesis of M(acac)n Complexes. Part II. Spectroscopy and Magnetic Suseptibility. Part III. NMR Spectroscopy (Magnetic susceptibility balance)
This is a junior level advanced course with organic and p-chem prerequisites. The course is an open ended student-designed pathway of a number of synthetic targets. Students design their own series of syntheses, decide which characterization methods are appropriate, monitor their own progress, carry out multiple tasks each day (synthesis, purification, and characterization) and write up their work as an experimental section of a journal article.
The possible syntheses include:
Bis(diphenylphosphino)methane
fac-[MnBr(CO)3(dppm)]
cis-mer-[MnBr(CO)2P(OPh)3(dppm)]
trans-[MnBr(CO)2P(OPh)3(dppm)]
Ferrocene
Salen(H2) and Co(salen)
YBa2Cu3O7-8
[(+)-Co(en)3][(+)-tart]Cl·5 H2O
(+)-Co(en)3]I3·H2O
(-)-Co(en)3]I3·H2O
Hexakis(4-nitrophenoxy)cyclotriphosphazene
M(acac)3 (M = Co, Cr, Mn, Fe, Cu)
At Hope, we teach a one-semester inorganic lab that is only required for students pursuing the ACS certification. This might change with the new ACS-CPT guidelines.
Students can take the lab in their junior or senior year, and they don't have to take it at the same time they're taking the lecture part of the course.
It is currently a synthesis-focused, project-based lab, although I hope to add a computational component next year.
The first project is the synthesis of a cobaloxime. I find this to be a good, simple example of the synthesis of a coordination compound, but with a bioinorganic twist. We use two different synthetic routes to add the alkyl substituent (reduction of cobalt followed by ox. add. of alkyl halide and Grignard addition to cobalt-halide) and they use a variety of alkyls. Each student is assigned one synthetic route and one alkyl. This lab introduces working with very forgiving air-sensitive compounds and NMR.
Then we do a longer project based on Grubbs chemistry, which includes a research-like component. Students begin by making and using a Grubbs catalyst. This part of the project is based on Ted M. Pappenfus,* David L. Hermanson, Daniel P. Ekerholm, Stacie L. Lilliquist, Megan L. Mekoli, J. Chem. Educ. 2007, 84, 1998. The supplementary material to that paper is so well written, that you can basically run with it in lab with minimal modification.
Finally the students propose and carry out a new reaction to try with their catalyst or a modification of the catalysis design.
Oh, and we also still do glassblowing in the lab. The students love it. It's one of the highlights of their chemistry training. I think they make three pieces in the first half of the semester and three in the second. We give prizes.
Another year rolls around and it's time to start thinking about inorganic lab again. But this year I have a new inorganic colleague who is a materials person, so I will get to learn new things! I want to keep the project-based approach and the research project, but now we should be able to introduce some new laboratory techniques that I am less familiar with.
I want to keep a coordination chemistry experiment, and while I'm getting tired of the cobaloxime lab, it does have biological connections which the students like, and it provides beautiful NMRs to analyze.
The Grubbs chemistry (see above) was fun and it led nicely into some research projects.
But I'm looking for new ideas!
So I'll pose the question again for our newer (and for our more mature) VIPEr users: What do you do in lab? What do you like? What would you like to change?
Joanne,
I made changes to my inorganic lab this semester. We have changed our curriculum for second semester GChem, and no longer discuss coordination chemistry. As a result, the students see coordination chemistry in my lab. The first part of the lab is coordination chemistry--reacting copper with glycine, which gives a very pretty powder blue color. I have the students collect IR data for their products and compare it to the IR reported in the 1950s. The second part of the lab focuses on research projects.