CHEMISTRY 324, SPRING 2000

INORGANIC CHEMISTRY LABORATORY

Dr. Joanne Stewart; Peale 205; ext - 7634; email - stewart@hope.edu

 

 

PROPOSED SCHEDULE, 1/13/00

 

DATE

CHEMISTRY

PRELAB

DUE DATES

Jan 13

intro, working with air-sensitive materials

Schlenk techniques, inert atmosphere glove box

 

Jan 20

make cobaloxime

overview of cobaloxime project

turn in copy of reagent table before lab

Jan 27

recrystallize cobaloxime, NMR, IR, mp analysis

Varian 400 MHz NMR

 

Feb 3

Finish cobaloxime analysis.  With partner, compare two routes to cobaloximes, compare NMR’s.

overview of Sn project

turn in table of proposed NMR assignments at end of lab

Feb 10

A.  make Li[N(SiMe3)2]

 

B.  resolve diamine

resolution of enantiomers, working with n-BuLi

cobaloxime report due before lab.

Feb 17

A.  isolate Li[N(SiMe3)2], NMR, mp analysis

 

B.  make derivative of resolved amine, chiral HPLC

chiral HPLC

 

Feb 24

A.  make Sn[N(SiMe3)2]2

 

B.  make Li[N(SiMe3)2]

 

A.  Li[N(SiMe3)2] results due

 

B.  turn in results on resolution of amine

March 2

A.  distill Sn[N(SiMe3)2]2, NMR

 

B.  isolate Li[N(SiMe3)2], NMR, mp analysis

vacuum distillation

 

March 9

A.  resolve diamine

 

B.  make Sn[N(SiMe3)2]2

 

A.  Sn report due before lab

 

B.  Li[N(SiMe3)2] results due

March 16

A.  make derivative of resolved diamine, chiral HPLC

 

B.  distill Sn[N(SiMe3)2]2

 

A and B.  Research proposal due before lab (one proposal for each pair of students)

March 23

spring break

 

 

March 30

catch up, prepare for research project

 

B.  Sn report due before lab

April 6

research project

 

 

April 13

research project

 

 

April 20

research project

 

 

April 27

Finish up, clean up

 

A and B.  Report on research project due before lab

 

 

 

WELCOME TO THE HOPE COLLEGE INORGANIC CHEMISTRY LABORATORY.  The course is designed to give you experience in the synthesis and characterization of molecules.  You will also have the opportunity to propose and carry out new reactions.  You are guaranteed an A if your work results in a chemistry publication in a professional journal!

 

Inorganic Chemistry Laboratory is a required course for ACS-BS Chemistry majors and an optional one for ACS-BS Biochemistry Emphasis and BA Chemistry majors.

 

Philosophy of the course:

 

The Inorganic Chemistry Laboratory will be an active, hands-on learning experience steeped in inquiry.  In a structured manner, students will propose and carry out experiments using modern inorganic techniques.  “Showing creativity” in solving problems is one of the desired student outcomes for the Chemistry Department, and this course will provide an opportunity for students and the Department to show that this learning goal has been met.

 

The goals for the course are to:

 

1.      Expand your experience with modern inorganic synthetic methodology.

 

2.      Expand your experience with modern instrumental techniques commonly used to characterize and study inorganic and bioinorganic materials.

 

3.      Develop higher skills associated with research, such as reading the inorganic and bioinorganic literature, designing experiments, analyzing data, and writing research proposals.

 

 

OFFICE HOURS:  I maintain open office hours and you should feel free to stop by and discuss any questions or concerns you have at any time.  You may also submit questions by email (stewart@hope.edu) or on ChemBoard (http://www.chem.hope.edu/chemboard).  Go to the Inorganic Chemistry part of ChemBoard and you will find the lab discussion at the bottom of the subtopics.  I will generally reply to questions the same day or the following morning.

 

GRADING:  Your grade will be based on three research reports written individually and one research proposal written with a partner.  There will also be a subjective component based on your general enthusiasm and adherence to safety concerns.

 

 

HONOR CODE

Academic integrity is assumed. Working with other students is encouraged, but this does not mean copying other’s work or using work completed in other years. Violations will be dealt with according to Hope College’s Code for Academic Integrity, as described in the official Hope College Catalog.

 

 

 

SAFETY, ENVIRONMENTAL, AND ECONOMIC CONCERNS:

 

1.      NEVER WORK ALONE IN THE LABORATORY.  You may work in the lab only when Dr. Stewart is present on the floor.  You may not work at night.

 

2.      SAFETY GLASSES OR GOGGLES MUST BE WORN AT ALL TIMES.  Glasses must have side shields.

 

3.      Wear a laboratory coat.  Sandals are not allowed in the lab.

 

4.      Eating, drinking, or smoking in the laboratory is prohibited.

 

5.      Learn the location and proper use of fire extinguishers, safety showers, and eyewashes.

 

6.      Learn the location of first aid materials.  Report accidents or injuries, even minor ones, promptly to the instructor.  The instructor must fill out an accident report form, even for minor problems.

 

7.      You will be working with some very reactive chemicals in this lab.  Be sure you are well versed in the proper techniques before handling them.  Disposable gloves are recommended for most labs.  Work in a hood when possible.  If chemicals come in contact with your skin, rinse the affected parts with water.  Wash your hands with soap and water when you leave the laboratory.  Never let chemicals come in contact with your eyes or mouth.  If by accident this occurs, wash affected areas with copious quantities of water and inform your instructor as soon as possible.

 

8.      Dispose of chemicals properly.  There will be different waste containers associated with each project.

 

9.      Broken glass must be discarded in the specially marked boxes in the laboratory.

 

10.  The equipment and glassware for this lab is very expensive.  Please use extra caution and tell the instructor if you break something, because replacements must be special ordered.

 

 

LABORATORY NOTEBOOKS

 

1.      Obtain a new permanently bound notebook.  The “Composition” style with gridded pages is a good choice.

 

2.      Leave two pages at the beginning of the notebook blank for a Table of Contents.

 

3.      All entries must be made in INK, not pencil.

 

4.      NEVER ERASE.  If you make a mistake, simply draw a single line through the error and initial and date it.  Leave the mistake such that it can still be read.

 

5.      NEVER REMOVE PAGES from the notebook.  If you want to redo a page, simply draw a large X through the page.

 

6.      MAKE ALL ENTRIES DIRECTLY INTO THE NOTEBOOK.  This means you.  Do not record masses, calculations, etc., on separate sheets of paper.

 

7.      Every page must have your name, the date, and the title of the experiment at the top.  Never leave blank pages to come back to later.

 

Before the lab, you must write a prelab similar to that required in Hope’s organic laboratory course.  Your prelab will be checked at the beginning of lab and you may not begin work until it is complete.  Your prelab should contain:

 

1.      Title of experiment, your name, and the date (on every page)

2.      Purpose of the experiment

3.      Chemical process to be investigated (balanced chemical reactions)

4.      Table of reagents: Compound, Mass or Volume used, MM, Density or Molarity if volume given, Moles, mp or bp.

5.      Flow diagram for synthesis

6.      Brief description or drawing of new or special equipment

7.      Reference to the source for the experimental procedure

8.      Calculation of theoretical yield

 

During and after the lab you should record:

9.      A description of the experiment written as the work is done in the laboratory

10.  A very brief summary of the results (What did you make?  What was the %yield?)

REPORT WRITING

 

For this course you will write three formal laboratory reports and one research proposal.

 

The reports will be written in the style and format currently used in American Chemical Society journals.  See, for example, Journal of the American Chemical Society (JACS) or Inorganic Chemistry.

 

Your report must contain the following clearly labeled sections:

·        Title, Name, Date

·        Introduction - should include some (referenced) background information, a statement of what experiment was carried out, and a rationalization for carrying out the study

·        Experimental - MUST be written with correct format, see sample report provided

·        Results and Discussion - brief description of what you did, results, what it means

·        Conclusions - final concise summary of your results, suggestions for future directions

·        Acknowledgements - often the payer of the bills is recognized, and anyone who provided helpful expertise or assistance.

·        References - references must be formatted correctly, see recent JACS for examples or ACS Style Guide.  They should be at the end of the paper.

 

All figures must have good figure captions written in complete sentences (below the figure) and all tables must have titles (at top of table) and footnotes (at bottom of table) giving any needed additional information.  Many scientists first “read” a paper by looking only at the figures and tables, so they need good captions and titles.

 

More hints and guidelines:

 

Reports should be written using complete sentences.  You should always use past tense, third person, passive voice.

 

Correct:            The reaction mixture was treated with...

Incorrect:          I treated the reaction mixture with...

Incorrect:          Treat the product with...

 

The verb react is intransitive.  The word treat may be used instead.

 

Correct:            The compound reacted with the Grignard reagent.

Correct:            The compound was treated with the Grignard reagent.

Incorrect:          The compound was reacted with the Grignard reagent.

 

Always include the amounts of reagents or products (grams and number of moles) and solvents (volume, usually in mL).  A decimal point should always precede a numeral

 

Correct:            0.036 mol

Incorrect:          .036 mol

 

Never begin a sentence with a number.  This sometimes leads to somewhat awkward constructions.

 

Correct:            Dimethylglyoxime (2.20 g, 19.0 mmol) was added to the solution.

Correct:            To the solution was added 2.20 g (19.0 mmol) of dimethylglyoxime.

Incorrect:          2.20 g (19.0 mmol) of dimethylglyoxime was added to the solution.

 

Compound adjectives are hyphenated.

 

Correct:            A 30-mL portion of the solution was placed in a 100-mL three-necked round-bottom flask.

However:         Add 30 mL of diethylether.

 

Write out the full name of all starting materials and products.  Molecular formulas may be used in place of the names of reagents and solvents, however do not begin a sentence with a formula.

 

The following abbreviations should be used (without periods, except where shown):

 

            boiling point                                                      bp

            gram(s)                                                 g

            degrees Celsius                                     °C

            hour(s)                                                             h

            infrared (spectrum)                                           IR

            liter(s)                                                               L

            literature                                                           lit.

            melting point                                                     mp

            milligram(s)                                                       mg

            milliliter(s)                                                         mL

            millimole(s)                                                       mmol

            minute(s)                                                          min

            mole(s)                                                 mol

            nuclear magnetic resonance (spectrum)  NMR

 

Three word-processing things you must know and use:

1.      You must use superscripts and subscripts appropriately.  Usually they are in a slightly smaller font (Word does this automatically); for example, Sn[N(SiMe3)2]2 or 6.02´1023.  In Word, highlight the desired letters or numbers and use Ctrl/= for subscript or Ctrl/Shift/= for superscript.

2.      You must use the appropriate degree symbol (°) when reporting temperature, not a superscripted “o.”  In Word go to Insert/Symbol... and you will find the degree symbol in several of the font choices.  Look in the Symbol font, for example.

3.      Use “non-breaking hyphens” when needed so that negative numbers are not wrapped away from their negative sign (meaning the negative sign is at the end of one line, and the number is at the beginning of the next).  In Word go to Insert/Symbol... and click the Special Characters tab.  You will find non-breaking hyphen in the list of choices.  The shortcut key is Ctrl/-.