Submitted by Chip Nataro / Lafayette College on Sat, 03/21/2020 - 12:56
Additional Authors
Lisa Bell-Loncella / University of Pittsburgh at Johnstown
My Notes
Categories
Prerequisites
First Semester Inorganic Chemistry / Foundation Course in Inorganic Chemistry
General Chemistry
Organic Chemistry
Corequisites
No Corequisites
Course Level
Second year
Upper Division/Graduate
Topics Covered
Bonding models: Discrete molecules
Descriptive chemistry
Electronic spectroscopy
Molecular structure
Organometallic chemistry
Physical methods / analytical techniques
Synthesis and reactivity
Visualization
Subdiscipline
Electrochemistry
Molecular Structure and Bonding
Organometallic Chemistry
Spectroscopy and Structural Methods
Description

This is the classic Chromatography of Ferrocene Derivatives experiment from "Synthesis and Technique in Inorganic Chemistry" 3rd Ed. (1986 pp 157-168) by R. J. Angelici. There are no significant changes from the experiment published in the book so details will not be provided. What is provided are links to some excellent videos showing the experiment and characterization data for students to work with. For the time being this will be a living document. Currently it has 1H, 13C{1H}, COSY, DEPT, HMBC, HSQC IR, UV-Vis, GC-MS and Cyclic Voltammetry raw data files for all compounds for students to work with. It also includes processed 1H, 13C{1H}, COSY, DEPT, HMBC, HSQC, IR, GC-MS and Cyclic Voltammetry data for all compounds. If anyone has any additional means of characterization they would like to include (say Mossbauer) please feel free to contact the author.

Attachment Size
Ferrocene raw NMR data: 1H, 13C, COSY and DEPT 4.31 MB
Ferrocene raw NMR data: HMBC 16.16 MB
Ferrocene raw NMR data: HSQC 26.98 MB
Ferrocene processed NMR data: 1H, 13C, COSY, DEPT, HMBC and HSQC 140.68 KB
Acetylferrocene raw NMR data: 1H, 13C, COSY and DEPT 4.6 MB
Acetylferrocene raw NMR data: HMBC 17.11 MB
Acetylferrocene raw NMR data: HSQC 27.85 MB
Acetylferrocene processed NMR data: 1H, 13C, COSY, DEPT, HMBC and HSQC 156.2 KB
Diacetylferrocene raw NMR data: 1H, 13C, COSY and DEPT 4.61 MB
Diacetylferrocene raw NMR data: HMBC 16.8 MB
Diacetylferrocene raw NMR data: HSQC 26.06 MB
Diacetylferrocene processed NMR data: 1H, 13C, COSY, DEPT, HMBC and HSQC 156.87 KB
GC-MS data for mixture of compounds in OLD format and MestReNova 3.91 MB
GC-MS data for mixture of compounds processed 188.74 KB
Cyclic Voltammetry of compounds (1.0 mM) in CH2Cl2 with NBu4PF6 (0.1 M) at Glassy Carbon. Needs correction of potentials. 120.56 KB
Cyclic Voltammetry of compounds (1.0 mM) in CH2Cl2 with NBu4PF6 (0.1 M) at Glassy Carbon. Corrected to make ferrocene 0 V.. 534.46 KB
Raw IR data for all compounds in CDCl3 466.97 KB
Processed IR data for all compounds in CDCl3 267.18 KB
UV-Vis data taken in CH2Cl2. 121.53 KB
Learning Goals

A student should get an appreciation for what doing this lab would be like by watching videos. In addition, the student will analyze the data provided and learn about the characterization of ferrocene, acetylferrocene and 1,1'-diacetylferrocene.

Equipment needs

Nothing.

The NMR data comes from a Bruker instrument and can be opened with TopSpin, MestReNova and perhaps other programs.

Implementation Notes

Like most everyone at this time this is going to be a trial by fire.

Web Resources
A very lab focused video from the Univ. of Sheffield
Video focused more on background material
Bruker Topspin for academia
MestReNova
Creative Commons License
Attribution, Non-Commercial, Share Alike CC BY-NC-SA