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Dr. Mark S. Delaney
Office: Kirkman 215 A
Research Lan: Kirkman 215
Phone: 337/475-5956
FAX: 337/475-5950

E-mail: or

Office Hours: 10am-11:50 am M-F, other hours by appointment

Course Description: Inorganic preparations. A macro-scale laboratory integrating synthetic techniques and characterization using gravimetric, spectrometric and other techniques of characterization.

Prerequisites: CHEM 301 and 302 and CHEM 301L and 302L; CHEM 391 (may be waived by instructor or department head).

Textbook:In-house lab manual for CHEM 412//513, provided to students for copying.

Course Objectives/Student Learning Outcomes: After completing the course the student will be able to:

This class consists of two three hour lab periods per week and one hour of lecture per week on different laboratory techniques.

Assessment Methods

Students will write reports on seven experiments performed during the semester. Each report is due two weeks after the experiment is finished. Each report will be worth 25 points. Six experiments will be from required choices with the sevent being an independent project, approved by the instructor. Grades for the reports will depend on how well the report is written, not on results of the experiment itself. There will be a final worth 75 points on the lecture portion of the class.

A breakdown of the grading is shown below:

6 reports on required inorganic preparations at 25 points each 150 points
1 report on independent project 25 points
Final on lecture material 75 points

The grading scale will be a 10 point scale as shown below:

100-90 A
89-80 B
79-70 C
69-60 D
59--0 F

Excused absences are allowed only for illness (with a doctor's excuse) and official university functions (band, athletics, field trips, etc.)

Lab reports for this class shall consist of an introduction, experimental section, results and discussion section and a conclusion. The format will be the same as that used bye the journal Inorganic Chemistry. An example article is contained in your lab manual.

Methods of Instruction: Instruction will consist of lectures (and possibly Balckboard lectures), and laboratory experiments.

Course and University Polcies:

Diversity Statement: Students should visit the MSU webpage at for information about diversity awareness and sexual harassment policies and procedures.

ADA Statement: Students with impaired sensory, manual, or speaking skills are encouraged and have the responsibility to contact their instructor, in a timely fashion, regarding reasonable accommodation needs. Such students should also contact The Officed of Services for Students with Disabilities at Kaufman Hall Rm. 119, Box 92904, Lake Charles, LA 70609, Phone: (337) 475-5916, 1-800-622-3352 ext. 5916, Fax: (337) 475-5878, email: for reasonable accommodation needs.


A. Introductory Experiment

I. Synthesis of Copper (I) Chloride

a. Familiarization with laboratory
b. Gravimetric methods

B. Template Reactions

Choice of

II. Synthesis of Manganese (II) Phthalocyanine

a. Characterization

1. UV-visible spectroscopy
2. Infrared Spec troscopy

b. Options

1. Repeat with other metals such as Cu
2. Choice of purificaton via Soxhlet extraction of via high temperature sublimation using a tube furnace


III. Synthesis of Cobalt (II) N,N'-disalicylidene-1,2-ethylenediamine (CoSALEN)

a. Characterization

1. Infrared spectroscopy

b. Options

1. Study of oxygen uptake cycle of CoSALEN

C. Air Sensitive Reactions

Choice of

IV. Synthesis of Ferrocene

a. Characterization

1. Gas chromatography to check purity of prepared cyclopentadiene
2. UV-vis to determine extinction coefficients for ferrocene.
3. Infrared spectroscopy

4. 1H NMR of cyclopentadiene, dicylopentadiene and ferrocene

b. Options

1. Choice of sublimation or recrystallization for purification
2. Friedel-Crafts alkylation or acylation of ferrocene


V. Preparation of Tetraethyltin

a. Characterization

1. Infrared spectroscopy
2. 1H NMR spectroscopy
3. GC-mass spectrometry

D. Inorganic Oligomers and Polymers

Choice of

VI. Synthesis of Zinc Halatopolymers with Maleic Acid

a. Characterization

1. Infrared spectroscopy
2. Optical microscopy
3. Differential scanning calorimetry

b. Options

1. Replace zinc with Mn, Fe (air sensitive procedures needed) or Co
2. Replace maleic acid with citraconic, or phthalic acids
3. Do a combination of 1 & 2.


VII. Synthesis of Dimethylsiloxane Oligomer and Polymers

a. Characterization

1. Infrared spectroscopy of prepared silicone cyclooligomers
2 1H NMR spectroscopy of prepared silicone cyclooligomers
3. GC-mass spectrometry of prepared silicone cyclooligomers

b. Options

1. Attempt polymerization of silicone cyclooligomers to high molecular weight poly(dimethylsiloxane)
2. Crosslink silicone cyclooligomers with boric acid to prepare bouncing putty (silly putty)

E. Crystal Growth

VIII. Methods for Crystallization of Inorganic Compounds

a. Methods

1. Use of seed crystal
2. Evaporative methods

b. Characterization

1. Determination of density of crystal via Archimedes method, displacement method and direct measurement

c. Calculations

1. Comparison to literature values for densities
2. Determination of approximate free volume in crystals of KAl(SO4)212 H2O, NaNO3 and PPh3 using effective ionic radii and thermochemical radii and experimentally determined densities

F. Pressure Reactions

Choice of

IX. Catalytic Hydrogenation of an Alkene using a Parr Hydrogentation Apparatus

a. Characterization

1. GC or GC-mass spectrometry to determine purity of starting alkene
2. GC or GC-mass spectrometry to determine amount of hydrogenation
3. Infrared spectrometry
4. 1H NMR of alkene and hydrogenated alkene

b. Options

1. Choice of alkene
2. Choice of various Pd and Pt catalysts


X. Polymerization of Ethylene using a Parr High Pressure Reactor

Choice of

1. Via Anionic Polymerization

a. Characterization

1. Determination of initial rate of polymerization via GC methods
2. Infrared spectroscopy of polyethylene
3. Differential scanning calorimetry (which can be used to estimate the approximate molecular weight of the relatively short polyethylene chains produced)

b. Options

1. Choice of various chelating tertiary diamines to use in conjunction with n-butyllithium


2. Via Ziegler-Natta Polymerization

a. Characterization

1. Infrared spectroscopy
2. Differential scanning calorimetry

b. Options

1. Choice of catalyst
2. Choice of supported or unsupported Ziegler catalysts
3. Choice of supports

G. Independent Project

The independent project must be approved by the instructor and such projects are viable only if the materials are readily on hand. The instructor reserves the right to refuse any project due reasons of potential hazards. Equipment which might be useful in the independent project in synthesis are listed below:

Crucible furnace
Glove box
Glove bags
Heating mantles
Muffle furnace
Nitrogen line with purification line
Parr High Pressure Apparatus
Schlenk glassware
Silicone oil bath
Standard organic glassware
Tube furnace
Ultrasonic bath

Instrumentation which might be useful in characterizing a product in your independent project is listed below:

Atomic absorption spectrometer
Differential scanning calorimeter
Gas chromatograph
Gas chromatograph-mass spectrometer
1H NMR spectrometer
Infrared spectrometer
Ultraviolet-visible spectrometer


Week 1 Notebook Keeping: Rules and Reasons
Week 2 Purification of Gas, Liquid and Solid Starting Materials
Week 3 Temperature Control, Low and High
Week 4 Very High Temperature Syntheses: Apparati made from the Proper Materials
Week 5 Air Sensitive Syntheses under Inert Atmosphere: Schlenk Techniques, Glove Bags and Glove Boxes
Week 6 The High Vacuum Line
Week 7 Separations: Distillations and Recrystallizations
Week 8 Separations: Chromatography
Week 9 High Pressure Apparatus
Week 10 Photochemical Apparatus
Week 11 IR, Raman and UV-Visible Spectroscopy
Week 12 Mass Spectrometry
Week 13 NMR Spectroscopy
Week 14 Thermal Techniques