Chem 454 Lab Syllabus – Spring 2010

TA: Anirban Das anirban.das@vandals.uidaho.edu

Office Hours: 10:25-12:25

 

Link To Chem 454 Lecture and Syallabus

Cheng Group Web Site

Note: To be updated throughout the semester. Last Update Dec. 8, 2010

·         Links     

·         Major Lab Write-up       

·         Minor Lab Write-up       

·         Special Assignment

 

Supplied Text: Chemistry Experiments For Instrumental Methods, DT Sawyer, WR Heineman, JM Beebe, John Wiley & Sons 1984

Laboratories:

Atomic Absorption Spectroscopy: See Chapter 9-3 of Lab Text. Instrument: Thermo S Series AAS

UV-Vis: Ocean Optics 2000, Chapter 6-1.

Fluorometry: Chapter 10-3, Hitachi F-2000

CG/MS: Agilent 5975 C MSD with 6890 GC

Other Labs --

HPLC: Various components with fixed  λ UV-Vis detector

Gas Chromatography: Chapter 12-3. Instrument: HP (Agilent) 5890/TCD

 

Important Dates

January                13 No Lab

                                20 Intro – Check in – Lab Assignments – Begin Major Lab – Make solutions required for calibration curves

                                27 Major Lab – Calibration Curves and Sample Run - Certification with unknowns

February              3 Major Lab – Sample Runs

                                10 Major Lab – Sample Runs and Clean up

                                17 Major Lab

                                24 Minor Lab - Major Lab Write Up Due

March                   3 Minor Lab

                                10 Minor Lab Due

                                17 Spring Break -- no lab

                                24 Begin Special Assignment – Proposal by groups using Powerpoint - Approval

March                  31-April 28 Special Assignment

May                       5 Dead week - Special Assignment Due

 

Links

UN Recommendations for the analysis of methamphetamine.

Agilent’s Web Site for the 5975 MSD This includes links to applications.

Thermo’s AA Spectrometry Web Page

 

Major and Minor labs will concentrate on GC-MS, GC-FID, AA and HPLC. Other labs may include ISE, FT-IR, UV-vis, and cyclic voltammetry

Major Lab Write-up.

Please follow the ACS format for Analytical Chemistry. Instead of the 5000 word limit Chem 454 lab reports should keep to 2500 words or less. Also include a brief error analysis with considerations taken for propagation and statistics in the Results and Discussion section. Please submit the reports as a MS Word .doc or .docx file to the TA’s email address. Please note the following taken from the pdf of Analytical Chemistry’s author guideline:

Text Consult the publication for the general writing style. Write for the specialist. It is not necessary to include information and details or techniques that should be common knowledge to those in the field.

 

General organization. Indicate the breakdown among and within sections with center heads and side heads. Results and Discussion follow the Experimental Section. Keep all information pertinent to a particular section and avoid repetition.

 

Abstract Abstracts (80-200 words) are required for all manuscripts and should describe briefly and clearly the purpose of the research, the principal results, and the major conclusions. Remember that the abstract will be the most widely read portion of the paper and will be used by abstracting services.

 

Introduction. The introduction should state the purpose of the investigation and must include appropriate citations of relevant, precedent work but should not include an extensive review of marginally related literature. If the manuscript describes a new method, indicate why it is preferable to older methods. If the manuscript describes an improved analysis of a substance, the competing methods must be referenced and compared. Absence of appropriate literature references can be grounds for rejection of the paper.

 

Experimental section. Use complete sentences (i.e., do not use outline form). Be consistent in voice and tense. For apparatus, list only devices of a specialized nature. List and describe preparation of special reagents only. Do not list those normally found in the laboratory and preparations described in standard handbooks and texts. Because procedures are intended as instructions to permit work to be repeated by others, give adequate details of critical steps. Published procedures should

be cited but not described, except where the presentation involves substantial modifications. Very detailed procedures should be presented in Supporting Information.

 

Safety considerations. Describe all safety considerations, including any procedures that are hazardous, any reagents that are toxic, and any procedures requiring special precautions, in enough detail so that workers in the laboratory repeating the experiments can take appropriate safety measures. Procedures and references for the neutralization, deactivation, and ultimate disposal of unusual byproducts should be included.

 

Results and discussion. The results may be presented in tables or figures; however, many simple findings can be presented directly in the text with no need for tables or figures. The discussion should be concise and deal with the interpretation of the results. In most cases, combining results and discussion in a single section will give a clearer, more compact presentation.

 

Conclusions. Use the conclusion section only for interpretation and not to summarize information already presented in the text or abstract.

 

References. References to notes/comments and to the permanent literature should be numbered in one consecutive series by order of mention in the text. The complete list of literature citations should be placed on a separate page, double-spaced, at the end of the manuscript. Reference numbers in the text must be superscripted. The accuracy and completeness of the references are the authors’ responsibility.

 

Examples of the reference format:

(1) Ho, M.; Pemberton, J. E. Anal. Chem. 1998, 70, 4915-4920.

(2) Bard, A. J.; Faulker, L. R. Electrochemical Methods, 2nd ed.;Wiley: New York, 2001.

(3) Francesconi, K. A.; Kuehnelt, D. In Environmental Chemistry of Arsenic; Frankenberger, W. T., Jr., Ed.; Marcel Dekker: New York, 2002; pp 51-94.

 

 

Minor Lab.

The authors of the corresponding Major lab will act as the consultant for the students of the minor labs. For the write-up, only the Abstract, Results and Conclusion sections will be reported. This should keep to a 500 word maximum.

Special Assignments

These labs will focus on projects in analytical/forensic chemistry that are of interest to the instructor, TA or to yourselves. A poster of the project will be presented at the end of the course. Suggested topics will be generated throughout the semester.