Chemistry 302Quantitative Analysis LaboratorySpring2012

Instructor: Dr. Jim BakerSection: 5TR (1:30 – 4:20 pm)Class/Lab: BEA 248/253

Office: Beauregard Hall 132 Phone: (985) 448-4576 Email:

Office Hours: MWF 2-5, Other times by appointment

Catalog Description: Chemistry 302. Quantitative Analysis Laboratory. 206. Pre/corequisite: Chemistry 300. The course includes determinations which illustrate the theories of gravimetric, volumetric, and instrumental analysis.

Prerequisite:C or better in CHEM 106/110Chemistry 300 is a co-requisite

Required Texts and Other Materials:

  1. Fundamentals of Analytical Chemistry, 8th ed, D. A. Skoog, D. M. West, F. J. Holler and S. R. Crouch, New York, NY, 2004.
  2. Laboratory notebook , (University Bookstore).
  3. Safety goggles, required (University Bookstore).
  4. Scientific or Graphing Calculator.
  5. Microsoft Excel or other appropriate spreadsheet software.
  6. Copies of handouts for the experiments are available through Blackboard. These handouts include suggested readings for each experiment. Chapter 2 contains information about the lab equipment and operations you will use in this lab.

Required Supplementary Readings: Posted on Blackboard

Course Goals: The student will develop the knowledge and abilities to allow them to:

1. Accurately and precisely complete the quantitative analysis of a wide variety of analytes.

2. Recognize and demonstrate proper laboratory technique.

3. Write a clear, concise lab report.

4. Demonstrate an understanding of the concepts involved.

Student Outcome Objectives:

  • Adept in the use of classical methods such as gravimetric, electrogravimetric, , precipitation titrations and acid/base titrations in a chemical determination.
  • Adept in the use spectroscopic methods such as atomic and molecular absorption spectroscopy and gas chromatographic methods to determine the amount of a substance in an unknown sample.
  • An ability to make accurate standard and reagent solutions.
  • Proficiency in the use of calibration techniques such as external standards and internal standards.
  • An ability to use statistics to interpret the results of the above determinations.
  • An ability to collect good data from an experiment.
  • An ability to analyze data from an experiment and to draw conclusions based on the results observed.
  • An ability to use Excel to analyze data from a chemical analysis.

The La. State Grade Level Expectations (GLE) for Chemistry (Grades 11/12) covered in this course can be found at

Course Content: Experiments (X) See attached calendar.

Preliminary Exercise 1: Treatment of Experimental Uncertainty

Preliminary Exercise 2: Measures of Density

X 1. Gravimetric Determination of Chloride in a Soluble Sample Ch. 37B, pp 1062-1064

X 2 Electrogravimetric Determination of Cu in an Ore Sample: 37K pp1098-1100; Handout

X 3 Fajans Volumetric Determination of Chloride: pp 356 – 8; Experiment 37D-2 pg 1075-1076. Handout

X 4 Volumetric Determination of Soda Ash: Ch 13, pp 732-737 See handout for procedure.

X 5 Spectrophotometric Determination of Iron.: Ch. 37N, 1104-1106, See handout for procedure.

X 6 Atomic Absorption Spectrophotometric Determination of Cu in Copper Ore: See handout for procedure.

X 7 Gas Chromatography of an Organic Mixture :Ch 24, 25 See handout for procedure.

Course Requirements: Safety: You are required to sign and follow a departmental safety contract. Other course requirements are specified in this syllabus.

Methods of Evaluation: Your overall grade will be obtained by adding the points you earn in each of the following categories: Lab Report and Unknown 100 points x 9 exercises. Final Exam: 100 Points Total = 1000 points.

Grading scale – A= 1000 900; B=899 800; C=799 700; D=699 600; F= below 599 points.

* Refer to attached grading scale and notebook guidelines.

2 PTS PERDAY WILL BE DEDUCTED FOR LATE LABReport Submission

Tentative Schedule

T1/20Check in. / Lecture on Lab Techniques

Th 1/25Preliminary Exercise #1 Stats calculations, Review Least Squares

T1/27Preliminary Exercise #2 Measures of Density

ROTATING SCHEDULE

Day / Date/Group / A / B / C / D
T / Jan. 24 / Check-in
Th / 26 / Prelim. Ex. 1
T / 31 / Prelim. Ex. 2
Th / Feb. 2 / X1 / X2 / X3 / X4
T / 7 / X1 / X2 / X3 / X4
Th / 9 / X1 / X2 / X3 / X4
T / 14 / X1 / X2 / X1 / X4
Th / 16 / X2 / X3 / X1 / X7
T / 21 / Mardi Gras Holiday
Th / 23 / X2 / X3 / X1 / X1
T / 28 / X2 / X3 / X1 / X1
Th / Mar. 1 / X2 / X5 / X4 / X1
T / 6 / X3 / X5 / X4 / X1
Th / 8 / X3 / X5 / X4 / X2
T / 13 / X3 / X4 / X4 / X2
Th / 15 / X6 / X4 / X7 / X2
T / 20 / X6 / X4 / X2 / X2
Th / 22 / X7 / X4 / X2 / X6
T / 27 / X5 / X7 / X2 / X6
Th / 29 / X5 / X6 / X2 / X3
T / Apr. 3 / X5 / X6 / X5 / X3
Th / 5 / X4 / X1 / X5 / X3
6-13 / Easter /Spring break
T / 19 / X4 / X1 / X5 / X5
T / 24 / X4 / X1 / X6 / X5
Th / 26 / X4 / X1 / X6 / X5
T / May. 1 / Check-out FinalExam

Makeup Policy: On mutual agreement with the instructor and subject to availability of equipment and/or reagents, make-ups are permitted during open lab periods in the student’s schedule.

Attachment A Grading Scale for Chem 302 Lab Reports

  1. Preliminary Experiments 1 and 2 and X6 require a formal report, containing,more or less, the following format.Reports are due one week after completion of the exercise.
  2. Introduction which expresses the background and purpose of the exercise.
  3. Experimental Procedure. Similar to Materials and Methods. Equipment, reagents and statistical or computational procedures and how they are used. This may be lengthy or may successfully cite well known methodologies without the need for lengthy detail, save for deviations from said methodologies.
  4. Discussion. This section should contain pertinent collected data, tables and conclusions reached after completion of the experiment.
  5. X1 through X6: Commercially prepared unknowns will be issued to you for X1-X5. Accurate concentrations have been supplied to your instructor by the manufacturer. Your experimental results and the calculations you turn in will determine the score you receive.
  1. X1 – X4: (Titrametric) Calculate and report the average and standard deviation of at least 3 replicate measurements. Your score for each of these experiments will be broken down as follows:

50 points for accuracy, I will compare the value you report to the true value by computing your part per thousand (ppt) deviation from the true value. 1ppt (0.1%) error will result in the loss of 1 point. For each and every additional 2ppt error an additional point will be subtracted.

20 points. for proper calculations using your experimental data. Reports submitted with faulty calculations will most likely not yield a solution for accuracy anywhere near satisfactory, hence a loss of 70 points + any points taken away for precision (see next). If this is the case you will be given the opportunity to repair your calculations with a loss of 10 points.

30 points for precision, that is the internal agreement of your results. Criteria exist for rejection of data (see chapters 5 and 6 in your text). Moreover, most experiments contain directions for setting up a trial run which is not to be considered in the final assessment.

  1. X5 X7: (Spectroscopy and Chromatography) Plot the standard results. Compute slope, intercept and standard error. Your score for each of these experiments will be broken down as follows:

30 points for accuracy, I will compare the value you report to the true value by computing your part per thousand (ppt) deviation from the true value. Each 5ppt (0.5%) error will result in the loss of 1 point.

40 points. for proper plotting of the data and calculations using the data. The same penalties regarding calculations for X1-X4 apply for these experiments. Failure to supply proper graphs will result in the loss of 20 points.

30 points for precision. Credit will be awarded or subtracted based upon the apparent reliability of your data.

  1. X6 (Atomic Absorption Spectrophotometry) Formal Lab Report. See (1) above

200 Points Half for the report, the remaining 100 points as indicated above for X5 and X7

  1. Final Exam 300 Points

Attachment B. NOTEBOOK ANDLAB REPORT GUIDELINES-

A. General Rules for Notebooks

1. The laboratory notebook must be a permanently bound book with alternating white and colored quadrille ruled sheets. The colored sheets will be used to make carbon copies of the original white sheets. The ORIGINAL white sheets are to be handed in as part of the lab report.

2. ALLDATA IS TO BE RECORDED IN INK DIRECTLY INTO THE NOTEBOOK!

a. Use a black ink pen (do not forget the carbon paper)

b. Label and date all entries.

c. An error should be lined through with a single horizontal line.

d. A single diagonal line should be drawn across any section, table or page that is to be disregarded, initialed, and explained. This includes completely blank pages.

3. Number all the pages in the notebook in the upper right hand corner of the page. The colored carbon copies must bear the same number as the white originals.

4. Fill in the title page (page i) and page ii.

5. Use page iii for the Table of Contents. The numbers are for each page. The table of contents should be maintained on a current basis at all times.

B. Notebook Format

Begin each experiment on a new page, use all pages consecutively, and use the following format: Failure to bring and record in your notebook will result in 1% credit subtraction per day.

  1. Title, Date, Purpose and Unknown Number:
  2. Experimental Plan:Provide a brief (less than 1/2 page) summary of the experimental procedure; cite the source of the experimental procedure.
  3. Materials and Methods: This section is the laboratory "diary" in which you write a step by step description of what you do in the lab. Number your steps. Make a sketch of the experimental apparatus. Record details such as: Name, manufacturer, model number and other identification (ID) for instrumentation, Chemical manufacturer, grade, lot number and expiration date, etc.;name and/or formula of solute(s) and solvent(s) used in solution prep, concentration, date prepared and preparer's initials. Once the details are recorded, you need not repeat them unless there is a change.
  4. Results: Record your results in labeled data tables. Enter and tabulate data as it is collected. Any observations are to be recorded here also. If the data for one particular step is to be collected over several days, leave enough space in the data table for subsequent entries. All tables and graphs must be titled and labeled sequentially. Use appropriate units.
  5. Calculations and Results Give one example of each type of calculation used in the experiment that has not been included in the previous section. In general, this section will deal with the calculation of the final results. Be sure to include all appropriate units. Whenever multiple samples of the unknown are analyzed, the sample standard deviation (s), the coefficient of variation (CV), and the 95% confidence interval should be calculated. Tabulate your results.
  6. Discussion/Conclusion (about 1/2 page in length) - Word process or type (12 pt. font)State your results and interpret or explain them in this section. Objectively evaluate the results in terms of their precision and accuracy. Briefly describe any sources of error that affected your results. If applicable, give the expected range for the analyte.

Academic Honesty Policy: Cheating or scholastic dishonesty will not be tolerated. In cases of academic dishonesty the instructor may dispose of the matter by invoking a maximum sanction of immediate expulsion from the course and the issuance of a failing grade.

Student Withdrawals: The last day to withdraw from the class is 4:00 March 4, 2012.

Academic Disabilities Policy: If you have a documented disability that requires assistance, you will need to register with the Office of Disability Services for coordination of your academic accommodations. The Office of Disability Services is located in Peltier Hall, Room 100-A. The phone number is (985) 448-4430 (TDD 449-7002).

Academic Grievances:The proper procedure for filing grade appeals or grievances related to academic matters is listed in Section 5 of the Code of Student Conduct and at the following link: http:

Continued Learning Following an Emergency:In order to make continued learning possible following an extreme emergency,

Students are responsible for:

  • reading regular emergency notifications on the NSU website;knowing how to use and access Blackboard (or university designated electronic delivery system);
  • being familiar with emergency guidelines;
  • evacuating textbooks and other curse material;
  • contacting faculty regarding their intentions for completing the course.

Faculty are responsible for:

  • their development and use of Blackboard (or designated) software;
  • having a plan for continuing their courses using only Blackboard and email;
  • continuing their course in whatever way suits the completion of the course best, and being creative in the course;
  • making adjustments or compensations to a student’s progress in special programs with labs, clinical sequences or the like only in the immediate semester following the emergency.

NOTE: This syllabus is not a contract and no part of it should be construed as such. The syllabus is subject to change. Students will be notified of these changes in a timely manner.