1. MWF 11:30-12:20, Rm 108, College of Business Administration
ANALYTICAL CHEMISTRY
CHEM 421/821, Spring 2013
MWF 11:30-12:20, Rm 108, College of Business Administration
COURSE OUTLINE
Instructor: Dr. Robert Powers
Office Labs
Address: 722 HaH HaH
Phone:
web page:
Office Hours: 10:30-11:30 am MWF or by Special Appointment.
Required Items:
(i) Chem 482 & 484 are prerequisites
(ii) Text: “Principals of Instrument Analysis”, 6/e D. A. Skoog, J. F. Holler and S R.
Crouch; Thomson, New York
(iii) Calculator for exams (TI-89 style or a simpler model)

2. Course Outlined (cont.)
Course Work:
Exam 1: pts. (Mon., Feb. 10)
Exam 2: pts. (Fri., Mar. 7)
Exam 3: pts. (Mon, Apr. 14)
Final: pts. (10-12, Wed., May 5)
Written Report: pts. (Fri., Apr. 18)
Problem Sets (8): pts. (various due dates)
Total: pts.
ALL PowerPoint presentations, and answer keys for the problem sets and exams will be posted on BlackBoard.
Grading scale: A+=95%; A=90%; A-=85%; B+=80%; B=75%; B-=70%;
C+=65%; C=60%; C-=55%; D=50%; D-=45%; F=40%

3. Course Outlined (cont.)
Class Participation
Reading assignments should be completed prior to each lecture.
You are expected to participate in ALL classroom discussions
Exams
All exams (except the final) will take place at 6 pm in Rm 105, College of Business Administration on the scheduled date.
The length of each exam will be open-ended. You will have as much time as needed to complete the exam.
Bring TI-89 style calculator or a simpler model, approved translator and text book (you will be able to use certain charts, tables and appendix)
A review session will take place during the normal class time.
ALWAYS SHOW ALL WORK!!!!

4. Course Outlined (cont.)
Problem Sets
Problem sets are worth either 15 or 20 points each and are selected from the questions/problems at the end of each chapter in the text.
You may work together in groups, but everyone must submit their own set of answers to the problem set.
Please feel free to visit me during office hours for assistance in answering the problem sets.
You must show all work to receive full credit.
Problem sets are due at the beginning of class on the due dates listed in the syllabus course schedule.
Late Problem sets will incur a 5 point penalty.
Problem sets will not be accepted after the next problem set due date has occurred or after the last day of class.

5. Course Outlined (cont.)
Problem Sets (cont.)
Students generally perform very well on the problem set, which provides a “grade cushion” to the more challenging Exams.
PLEASE DO THE PROBLEM SETS!
DO NOT USE THE INTERNET, ANSWER KEYS OR SOLUTION MANUALS TO COMPLETE YOUR PROBLEM SET.
Failure to comply will result an automatic zero score for ALL problem sets.
You will receive a zero out of the possible 150 points
Penalty will occur for a single infraction.
A single problem on a single problem set – no exceptions.

6. PAPER ON INSTRUMENTAL METHODS
Paper General
4-5 pages single space text
Additional pages for figures, references
12 pitch font
Double spacing between paragraphs and headings
Paper Topic
Instrumental method
Principals behind technique
How the technique is used
Kind of instrumentation
What samples are used
Advantages/disadvantages

7. PAPER ON INSTRUMENTAL METHODS
Application of instrumental method
Brief review of the properties of sample of interest
How these properties are used to analyze sample
What types of techniques are available
Advantages/disadvantages
Source of ideas
Journals: Analytical Chemistry, Analytical Biochemistry Trends in Analytical Chemistry(TrACs), C&E News, Science, Nature
Grading (50 points total)
Content
Clarity of Presentation
Comprehension of material
Paper topic needs to be approved by Monday, March 10th
Due Date: 11:30 am, Friday April 18th

8. PAPER ON INSTRUMENTAL METHODS
Your Paper is Not a “Cliff” Notes Summary of a Scientific Journal Article
Write the paper in a manner that explains the technique or application to a colleague or friend
Use Specific Data and/or Comparisons
Examples:
Poor – “mass spectrometry is very sensitive”
Excellent – “mass spectrometry has very high femtogram limits of detection compared to the micrograms required by NMR.
Use Figures within the text
It is much easier to describe a concept or results by referring to and describing the details of a figure
DO NOT PLAGIRAZE!
Plagiarism will result in an automatic failing grade and the incident of academic dishonesty will be reported to the Dean of Students.

9. Lecture Topics Date Chapter Topic
I. Introduction to Analytical Chemistry
Jan 13 Chap 1 Introduction
II. Spectroscopic Methods
Jan 15 Chap 6 Introduction to Spectroscopy
Jan 17 Chap 6
Jan 22 Chap 7 Instrumentation for Spectroscopy
Jan 24 Chap 7
Jan 27 Problem Set #1 due
Jan 29 Chap UV/Visible Molecular Absorption Spectroscopy
Jan 31 Chap 13-14
Feb 3 Chap 13-14
Feb 5 Chap Molecular Luminescence Spectroscopy
Feb 7 Problem Set #2 due
Feb 10 EXAM 1
Feb 12 Chap Infrared Spectroscopy
Feb 14 Chap 16-17
Feb 17 Chap Raman Spectroscopy
Feb 19 Problem Set #3 due
Feb 21 Chap Atomic Spectroscopy
Feb 24 Problem Set #4 due
Feb 26 Chap Introduction to Chromatography
III. Separation Methods
Feb 28 Chap Gas Chromatography
Mar 3 Chap 27
Mar 5 Problem Set #5 due
Mar 7 EXAM 2

10. Lecture Topics Date Chapter Topic
Mar 10 Chap Liquid Chromatography/Paper Topic Approvals
Mar 12 Chap 28
Mar 14 Chap Other Separation Methods
Mar 17 Problem Set #6 due
IV. Electrochemical Methods
Mar 19 Chap Introduction to Electrochemistry
Mar Chap 22
March Spring Break
Mar 31 Chap 22
Apr 2 Chap Potentiometry
Apr 4 Chap 23
Apr 7 Chap Coulometry
Apr 9 Chap Voltammetry
Apr 11 Problem Set #7 due
Apr 14 EXAM 3
V. Other Techniques
Apr 16 Chap NMR
Apr 18 Chap 19 Instrumental Methods Paper Due
Apr 21 Chap 19
Apr 23 Chap 19
Apr 25 Chap 11,20 Mass Spectrometry
Apr 28 Chap 11,20
Apr 30 Problem Set #8 due
May Review Session
May 5 FINAL EXAM

11. Introduction to Analytical Chemistry
Background
A.) ANALYTICAL CHEMISTRY: The Science of Chemical Measurements.
B.) ANALYTE: The compound or chemical species to be measured, separated or studied
C.) TYPES of ANALYTICAL METHODS:
1.) Classical Methods (Earliest Techniques)
a.) Separations: precipitation, extraction, distillation
b.) Qualitative: boiling points, melting points, refractive index, color,
odor, solubilities
c.) Quantitative: titrations, gravimetric analysis
2.) Instrumental Methods (~post-1930’s)
a.) separations: chromatography, electrophoresis, etc.
b.) Qualitative or Quantitative: spectroscopy, electrochemical methods,
mass spectrometry, NMR,
radiochemical methods, etc.

12. How Do We Answer or Address These Questions?
CHOOSING AN ANALYTICAL METHOD
What Factors to Consider:
What type of information does the method provide?
What are the advantages or disadvantages of the technique versus other methods?
How reproducible and accurate is the technique?
How much or how little sample is required?
How much or how little analyte can be detected?
What types of samples can the method be used with?
Will other components of the sample cause interference?
Other factors: speed, convenience, cost, availability, skill required.
How Do We Answer or Address These Questions?

13. Two types of error: random or systematic
CHARACTERISTICS OF AN ANALYTICAL METHODS
Accuracy: The degree to which an experimental result approaches the true or accepted answer.
Ways to Describe Accuracy:
Error: An experimental measure of accuracy. The difference between the result obtained by a method and the true or accepted value.
Absolute Error = (X – m)
Relative Error (%) = 100(X – m)/m
where: X = The experimental result
m = The true result
All Methods, except counting, contain errors – don’t know “true” value
Two types of error: random or systematic

14. CHARACTERISTICS OF AN ANALYTICAL METHODS
Random Error: results in a scatter of results centered on the true value for repeated measurements on a single sample.
Systematic Error: results in all measurements exhibiting a definite difference from the true value
Random Error
Systematic Error
plot of the number of occurrences or population of each
measurement (Gaussian curve)

15. CHARACTERISTICS OF AN ANALYTICAL METHODS
Precision: The reproducibility of results. The degree to which an experimental result varies from one determination to the next.
Precision is related to random error and Accuracy is related to systematic error.
Illustrating the difference between “accuracy” and “precision”
Low accuracy, high precision
Low accuracy, low precision
High accuracy, low precision
High accuracy, high precision

16. CHARACTERISTICS OF AN ANALYTICAL METHODS
Ways to Describe Precision:
Range: the high to low values measured in a repeat series of experiments.
Standard Deviation: describes the distribution of the measured results about the mean or average value.
Absolute Standard Deviation (SD):
Relative Standard Deviation (RSD) or
Coefficient of Variation (CV):
where: n = total number of measurements
Xi = measurement made for the ith trial
= mean result for the data sample

17. CHARACTERISTICS OF AN ANALYTICAL METHODS
Response: The way in which the result or signal of a method varies with the amount of compound or property being measured.
Ways to Describe Response:
Calibration Curve: A plot of the result or signal vs. the known amount of a known compound or property (standard) being measured.

18. CHARACTERISTICS OF AN ANALYTICAL METHODS
Parameters used to Describe a Calibration Curve: S = mc + Sbl
S – measured signal
c – analyte concentration
Sbl – instrument signal for blank
Sensitivity: calibration sensitivity = slope (m) of calibration curve.
analytical sensitivity (g) = slope (m)/standard deviation (Ss)
ability to discriminate between small
differences in analyte concentration.
Slope and reproducibility of the
calibration curve.
Method A
Method B

19. No method is totally free from interference from other species.
Selectivity: degree to which the method is free from interference by other
species in the sample
No method is totally free from
interference from other species.
Selectivity coefficient (k):
kB,A = mB/mA
Relative slopes of calibration curves indicate selectivity:
S = mA(cA + kB,Acb) + Sbl
Species A
Species B
Interested in detecting species A, but signal will be a combination of signal
from the presence of species A and species B.

20. Signal-to-noise Ratio (S/N):
Limits of Detection (cm ): (minimum analyte signal (Sm) - mean blank signal( ))/slope(m)
minimum/maximum concentration or mass of analyte that can be detected at a known confidence level.
Signal-to-noise Ratio (S/N):
Noise: random variation in signal or background
Signal: net response recorded by a method for a sample
(Note: a value of S/N = 2 or better is considered to be the minimum ratio needed for the reliable detection of a true signal from a sample.)
Estimate S/N:
Multiple determination of blank samples.
Estimation of best-fit to calibration curves
signal
noise

21. Dynamic Range: linear region of calibration curve where the lower limit is ten times the standard deviation of the blank.
LOQ - limit of quantitation
LOL - limit of linearity
Concentration (mM)

22. Glucose Concentration, mM
Example 1: The data in the table below were obtained during a colorimetric determination of glucose in blood serum.
A serum sample gave an absorbance of Find the glucose concentration and its standard deviation, calibration sensitivity, detection limit and dynamic range.
Glucose Concentration, mM
Absorbance, A
0.0
0.002
2.0
0.150
4.0
0.294
6.0
0.434
8.0
0.570
10.0
0.704