Instrumental Analysis, Fall 2015

Materials for Fall 2015

AM lab Turnitin : 10395698, password: stanislaus

Calendar for Fall 2015

Final Poster Session Requirements
Poster Session Rubric

Assigned reading and practice problems

Dr. Russell's Practice Problems & Materials
Chapter 7, Problems 1, 2, 8, 9, 12, 13, 14, 18
Chapter 13, Problems 1-9
Chapter 14, Problems 8, 9
Chapter 26: 1-3, 8, 10-15, 17, 20, 21
Chapter 27: 1, 3, 6-11, 13-16, 20-22, 26, 26
Chapter 28: 2-6, 8, 10, 11, 13, 14, 15, 16, 18, 19
Mass spec interpretation guidelines

Isotope Pattern Tables
Dr. Stone's Assignments and Practice Problems
Dr. Stone's Assignments and Practice Problems
Introduction to FT-IR
Water Vibrations
Carbon dioxide vibrations
Introduction to IR at Cal Tech
Video on ATR by Pike Industry

Must see: Tutorials and Exercises from the Text Be sure to watch the NMR videos and practice the Fluorescence questions on this site.
Watch this video about LASERs
Fluorescence: Chapter 15: 2,3,4,5,6,9
IR, FT: 204-207
IR, Michelson Interferometer: Chapter 7: read pages 208-211, watch simulation on textbook website: Tutorials and Exercises from the Text, do Chapter 7 problems: 22,23
Excellent IR resource Some of these sample spectra will be on the exam.
Tutorial on IR spectra interpretation
IR: Read pages 439-443, 449-452 in Chapter 16, and do problems: 1-9, 12, 13
IR: Read pages 459-469, 471-472 in Chapter 17 and do problems: 2-5, 8
Raman: Read pages 481-488 in Chapter 18 and do problems: 1-3
NMR: Chapter 6: 2-5
NMR: Chapter 19: 1-42
NMR Spectroscopy at U. of Wisconsin This site has some good practice problems for NMR spectra.
NMR resources:

  • Worksheet handed out in class, bring completed worksheet on Tuesday, October 27th.
  • More NMR practice
  • Even More NMR practice
  • 2D NMR
  • 2D NMR examples are in this final exam. If you are given the labelled structure, you should be able to read the COSY and HMQC data to determine connectivities and make assignments. (Which peak goes with which proton or carbon.)

Searching the Literature

Powerpoint file used in class.


Build a Spectrophotometer

Lab Safety

Lab Liability Release Form: You must read this and sign the form provided in lab prior to starting lab work.

General Lab Safety Policy

Fall 2015 Experiments

1. UV/VIS: 2 component mixture, Due Date: Sept 15th
Procedure, Grading Rubric

2. IR: unknown functional group determination, Due Date: October 1
Procedure, Grading Rubric

3. UV/VIS Method Development, Due Date: Oct 15th
Lab instructions, Lab 3 Rubric, Ascorbic acid for reduction of iron(III)

4. IR: Use IR to develop a method to quantitate OTC active ingredients, Due Date: Oct 29th
IR spectroscopy for Quantitating OTC drugs or go here: IR spectroscopy for OTC drugs and here is the Grading Rubric

5 & 6. NMR: Extraction/purification of a known compound from a crude mixture NMR Spectral Analysis. Due on Nov 19th
Important information: Make sure that you use deuterated solvents. Check your sample solubility in non deuterated solvents (they are much cheaper), but submit your sample in only deuterated solvent. The machine requires deuterium to find the lock signal. Also if your solvent has protons, your sample will be a needle in a haystack. Procedure, You will need to download the software from JEOL to process your 1D spectra (integrate, determine coupling constants, expand to determine multiplicity.) JEOL software instructions
Note: We have a 500mHz JEOL spectrometer that uses Eclipse+ software. You only want to process data. It can take several days to get approval for the software. Please start early. Here is the Grading Rubric

7. HPLC: Separation and quantitation of caffeine and theobromine from chocolate. Due Date: Nov 30th
Procedure, HPLC Rubric

8. GC: Method development for mixture separation quantitation in an unknown , Dec 3rd

9. Mass spectrometry: Fragmentation of a known peptide, Due Date: Dec 10th
Procedure to be posted, Grading Rubric to be posted

10. Mass spectrometry: Identification of an unknown protein via proteomics/mass spec. Due Date: Dec 10th
Procedure to be posted, Grading Rubric to be posted

Links to Useful information

Basics of NMR by Dr. Joseph Hornak
COSY NMR video

Old Exams

Exam 1 from 2013
Exam I from 2014
Exam Questions based on IR spectroscopy
Exam 1 from 2006
Practice UV-Vis Exam
NMR and IR exam from 2014
NMR exam from 2008
Practice for NMR Exam Questions
Practice with the Tutorials and Exercises from the Text

Experiments from previous years
UV-VIS: Determination of a two component mixture. Grading Rubric
IR Experiment Determination of Functional Groups by IRRubric for Functional Groups
IR Experiment:Quantitation of Analgesics. Rubric for IR Quantitation of Analgesic

  • References for IR Quantitation
  1. A Validated Method for the Quantitation of Ciprofloxacin Hydrochloride Using Diffuse Reflectance Infrared Fourier Transform Spectroscopy
  2. Diffuse Reflectance Must Read
  3. Characterization and Quantitationof Aprepitant Drug Substance Polymorphs by Attenuated TotalReflectance Fourier Transform Infrared Spectroscopy.

UV-Vis and Fluorescence Quantitation of Bis Phenol A.Rubric
NMR Lab Procedure: The process of obtaining a clean spectrum
Rubric for NMR Lab

GC Experiment Rubric for GC lab
HPLC Procedure:Rubric for HPLC lab
HPLC Method Conditions Paper
Mass spec lab procedure
Mass spec lab rubric

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