Chemistry 302 Quantitative Analysis Laboratory Spring 2010

Instructor: Darcey Wayment Section: 5TR (1:30 – 4:20 pm) Class/Lab: PEL 230/226 Office: PEL 257F Phone: (985) 448-4398 Email:[email protected] Office Hours: M,F 11-12, T, Th 9:30-10:30, W 4:00-5:00; Other times by appointment

Catalog Description: Chemistry 302. Quantitative Analysis Laboratory. 2-0-6. Prerequisite or co requisite: Chemistry 300. The course includes determinations which illustrate the theories of gravimetric, volumetric, and instrumental analysis. Pre or co requisite: Chemistry 300 Required Texts and Other Materials: Fundamentals of Analytical Chemistry, 8th ed, D. A. Skoog, D. M. West, F. J. Holler and S. R. Crouch, New York, NY, 2004. Scientific or Graphing Calculator is recommended plus passing familiarity with computer spreadsheet software. A laboratory notebook and safety goggles are required and can be purchased in the University Bookstore. Copies of handouts for some experiments will either be provided or 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 Content: Experiments (X) See attached calendar. Preliminary Exercise 1: Treatment of Experimental Uncertainty Preliminary Exercise 2: Measures of Density Reading assignment: Selected sections on text CD, Documents/Selected Methods-Chapter 37 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= 100 - 90 %; B=89 - 80%; C=79 - 70%; D=69 - 60%; F= below 59% * Refer to attached grading scale and notebook guidelines. NOTE: 2 PTS PER DAY WILL BE DEDUCTED FOR LATE LAB Turn-In 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. Attendance Policy: Attendance is mandatory. A total of two (2) unexcused absences will result in the student being dropped from the class with a grade of "F". 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. Tentative Schedule Th, 1/21 Check in. Lecture on Lab Techniques T, 1/26-28 Preliminary exercise #1 Stats calculations Review Least Squares Th, 1/28 Preliminary Exercise #2 Measures of Density (Continues on page 2)

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 1 ROTATING SCHEDULE Special Instructions Date/Group A B C D T, 2/2 X2 X1 X1 X3 X1: Bring crucibles to a constant weight on the first scheduled Th, 2/4 X2 X1 X1 X3 day of this lab. Report these results by end of class. NaCl T, 2/9 X2 X1 X1 X3 standard and unknowns can be left in the oven to dry st nd Th, 2/11 X2 X1 X1 X6 between 1 and 2 day of lab work. Th, 2/18 X1 X2 X3 X6 X2: Secure unknown and electrodes the lab period prior to your T, 2/23 X1 X2 X3 X1 start date. Clean the electrodes, dry and weigh them before Th, 2/25 X1 X2 X3 X1 you depart. Keep the electrodes in your drawers. CuO may T, 3/2 X1 X2 X4 X1 be kept in the drying oven between lab periods Th, 3/4 X3 X5 X4 X1 X3: Place recommended quantity of 1° standard NaCl in the T, 3/9 X3 X5 X4 X2 drying oven on the lab period before you begin. Determine Th, 3/11 X3 X5 X4 X2 the reproducibility of your titration data for both known Th, 3/18 X4 X3 X5 X2 and unknown runs. Have your instructors approval of the T, 3/23 X4 X3 X5 X2 results before leaving class Th, 3/25 X4 X3 X5 X5 T, 3/30 X4 X4 X2 X5 X4: Secure unknown and 1° standard the lab period prior to T, 4/9 X6 X4 X2 X5 your start date. Dry both between lab periods. Following T, 4/13 X6 X4 X2 X7 the titration of your unknown, and before you leave the st Th, 4/15 O O O O lab, plot results and 1 derivative using Excel. Have your Th, 4/20 X5 X4 X7 X4 instructors approval of the results before leaving class Th, 4/22 X5 X7 X2 X4 X5: Before leaving lab, plot results using Excel. Have your T 4/27 X5 X6 X6 X4 instructors approval of the results before departing Th, 4/29 X7 X6 X6 X4 X6: No solid unknown will be issued. Give your instructor a T, 5/4 O O O O cleaned 250 mL volumetric flask. Th, 5/6 Check out, Final Exam

Student Withdrawals: The last day to withdraw from the class is 4:00 Wednesday, March 31, 2010.

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.

Attachments: A Grading Scale, B. Notebook and Lab Report Guidelines, C. ACS Standards and Objectives 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).

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. learn proper sampling technique in instrumental analysis 4. write a clear, concise lab report. 5. demonstrate an understanding of the concepts involved. Student Outcome Objectives: The student will attain the following objectives developed by the Division of Analytical Chemistry of the American Chemical Society (ACS) and listed at : http://www.chemistry.org/portal/a/c/s/1/acsdisplay.html?DOC=education%5Ccpt%5Cts_anlchem.html

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 2 The successful student will:  Understand the distinction between qualitative and quantitative goals of determinations  Understand comparison and critical selection of methods for elemental and molecular analyses  Apply knowledge of sampling methods for all states of matter  Understand statistical methods for evaluating and interpreting data  Understand concepts of validation of data and experimental design  Understand sources of error in chemical and instrumental analysis  Understand interferences in chemical and instrumental analysis  Understand theory and operational principles of analytical instruments  Demonstrate competence with computer-based data acquisition systems for analytical instruments  Understand the concept of instrument calibration  Demonstrate a fundamental understanding of the principles of and instrumentation for atomic and molecular spectrometry, chromatography, and electroanalytical methods.  Understand basic concepts of stoichiometry and basic chemical reactions involving analytes and ordinary reagents  Understand the importance to quantitation of equilibrium and kinetic aspects of chemistry  Understand concepts of availability and evaluation of analytical standards  Understand standardization methodology

The La. State Grade Level Expectations (GLE) for Chemistry (Grades 11/12) covered in this course can be found at http://www.doe.state.la.us/lde/ssa/1842.html#Chemistry.

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:www.Nicholls.edu/documents/student_life/code-of_conduct.pdf

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 sue 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.

This syllabus is provided solely for informational purposes and as a guide. It is not a contract and no part of it should be construed as such.

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 3 Attachment A Grading Scale for Chem 302 Lab Reports 1. Preliminary Experiments 1 and 2 require a formal report, containing, more or less, the following format. Reports are due one week after completion of the exercise. a. Introduction which expresses the background and purpose of the exercise. b. 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. c. Discussion. This section should contain pertinent collected data, tables and conclusions reached after completion of the experiment. 2. 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. a. 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. b. 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.

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 4 Attachment B. NOTEBOOK AND LAB REPORT GUIDELINES- Refer to the Notebook Checklist Rubric (Attachment B).

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. ALL DATA 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 and Purpose 2.) Experimental Plan Provide a brief (less than 1/2 page) summary of the experimental procedure, cite the source of the experimental procedure. 3.) Procedure and Data 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. 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. 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.) 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 a set-up with 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. 5.) Discussion/Conclusion (about 1/2 page in length) - Word process or type (12 pt. font) Interpret or explain your results 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.

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 5 LAB REPORTS:

Assemble the lab report as follows:

1. Cover sheet - Use the Report Form. 2. Notebook pages 3. Regular paper - Discussion / Conclusion - Word processed or typed 4. Notebook Rubric or Checklist (green)

When and how To Use Figures and Illustrations Figures can play a major role in highlighting and clarifying results and data. Appropriate, well-drawn figures can substantially increase comprehension of the text and can convey trends, comparisons, and relationships more clearly than text. However, figures that do not clarify the discussion but merely repeat data already presented in text, and figures that are poorly presented not only decrease comprehension, but also cause confusion. Combining curves that have the same set of axes saves time, space, and money, but do not put more than four or five curves in one set of axes. Leave sufficient space between curves; they should not overlap so much that the symbols are indistinguishable. Keep the figure compact; have axes only long enough to define the curve. For example, if the highest point on the curve is 14, then 15 should be the highest axis label. Furthermore, the origin or lowest point on the axes does not have to be zero. For example, if the lowest point on the curve is 4, then 3 should be the lowest axis label. Put grid marks on the axes to indicate the positions of the numbers. Label the axes with the parameter or variable being measured, the units of measure, and the scale. Use initial capital letters only, not all capitals. Place the units of measure in parentheses. Place all labels outside the axes and parallel to them. Letters and numbers should read from left to right and from bottom to top. Do not place arrowheads on the ends of the axis lines; simple, straight lines are adequate. Use only two axes, one horizontal and one vertical; do not draw the top horizontal and right vertical lines to make a box. Keep the illustration clear and simple. Keep wording to a minimum. Leave clear margins of at least 1 inch (2.5 cm) on all sides of the figure. Usually, computer-generated figures are preferred, but avoid using the "auto-scaling" feature of most software. You should choose a scale that uses as much of a full page within 1 inch margin limit) as possible and yet makes the graph easy to read. Avoid using 3,6,9 etc. when setting up your scale. How To Number and Cite Figures Number figures sequentially with Arabic numerals, in order of discussion in the text. Every figure must be discussed in the text; refer to them as "Figure 1", "Figure 2", etc. Figure Captions Every figure must have a caption that includes the figure number and a brief description, preferably one or two sentences or descriptive phrases. The caption should be understandable without reference to the text and should not include new material that is not in the text. Use similar wording for captions of related figures. Generally, put the keys to symbols in the caption, not in the artwork, where they tend to give a cluttered appearance. Make sure that the symbols and abbreviations in the caption agree with those in the figure itself and in the text. Credit lines for figures reproduced from previously published work must appear at the end of the caption. For example, "(Reproduced with permission from ..... Copyright 1985, Publisher.)"

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 6 Tables (Note: If a table is given in the experimental handout, use it as a guide only. Record all data directly in the lab notebook.) When To Use Tables Use tables when the data are precise numbers that must be presented, when there are too many to be presented clearly as narrative, or when more meaningful interrelationships can be conveyed using them. Tables should supplement, not duplicate text and figures. How To Construct Tables A table should consist of at least three columns, and the center and right columns must refer back to the left column. If you have three columns, but they do not relate to each other, perhaps the material is really a list of items and not a table at all. Tables should be simple and concise, but if you have many small tables, consider combining some. Combining is usually possible when the same column of data or information is repeated in separate tables. Use consistent wording for all elements of similar or related tables. Use symbols and abbreviations that are consistent among tables and between tables and text. Title Every table must have a brief title describing its contents. The title should be complete enough to be understood without referring to the text, and it should not contain new information that is not in the text. Put details in footnotes, not in the title. Column Headings Every column must have a heading that describes the material below it. Be as succinct as possible, keep headings to two lines, and use abbreviations and symbols. Define nonstandard abbreviations in footnotes. Name the parameter being measured and indicate the unit of measure after a comma. A unit of measure alone is not an acceptable column heading. Information that describes all of the columns belongs in a general footnote. Columns Usually, the leftmost column is the stub or reading column. All other columns should refer back to it. Stub entries should be consistent with the text as well as logical and grammatically consistent with each other. Main stub entries may also have sub-entries, which should be indented. Columnar information can be aligned in four different ways: on the left, the right, on the decimals, or centered. Words are usually aligned on the left, and numbers are usually aligned on the decimals. Always incorporate a zero before the decimal point if a number is less than one and scientific notation isn’t necessary. Groups of numbers connected by plus- minus signs and ranges of numbers connected by dashes can also be usually aligned on the symbols and centered in the column width. Do not use ditto marks or the word "ditto". Define all nonstandard abbreviations in footnotes. Try not to have any one entry much longer than all the others. Place any explanatory material for specific entries in footnotes. Be sure that all of the columns are really necessary. If there are no data in most of the entries of a column, it probably should be deleted and replaced with a general footnote or, if the entries in the entire column are the same, the column should be replaced with a footnote that says "in all cases, the value was x" or whatever is appropriate. Footnotes Footnotes include explanatory material referring to the whole table and to specific entries. Information that should be placed in general footnotes referring to the whole table is the following: units of measure that apply to all entries in the table, explanations of abbreviations and symbols used frequently throughout the table, details of experimental conditions if not already described in text or if different from the text, sources of data, and other literature citations. Examples of information that should be placed in specific footnotes are as follows: units of measure that are too long to fit in the column headings, explanations of abbreviations and symbols used with one or two entries, statistical significance of entries, experimental details that apply to specific entries, and different sources of data. How To Number and Cite Tables Number the tables sequentially with Arabic numerals, in order of discussion in the text. Like figures, every table must be cited in the text. SOURCE: The ACS Style Guide for Authors, J.S. Dodd, Ed. ACS Publications, Washington, D.C. , 1986

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 7 NAME______EXP. No. _____ Short Title_____Date______

Successful Scientific Notebook Keeping The practicing scientist, whether they be chemist, physicist, biologist or any discipline in- between succeed or fail on the strength of their ability to interpret their lab work. Attention to detail is paramount, both during the collection of data and in its subsequent scrutiny. It happens all the time. People see important things, fail to write down what they see and then forget all about it. Most of the time you don’t even think about it until you forget an important date. Scientists pride themselves on their ability to store and sort through seemingly unrelated numbers. It’s not until you really sit down and start to think about your experiences that you can finally start to make sense of them. Faulty memories lead to faulty conclusions. Enter the journal, or lab notebook. Think about how you set the thing up. Start organizing before you start writing and always have it on hand during lab. Whatever you see, smell, think or measure during lab may wind up being significant, so keep a record of everything. Below are some guidelines, including a general rubric or protocol..

A. Title Page (i.e. Course number and Title) Data tabulated B. Table of Contents Data tables numbered, titled C. General Format for each day Data table headings clear Units included in all data Student name & Experiment # on each page Correct sig. figs. Number and date Every Page, Black ink, NO PENCIL 4. Results – Calculations & Graphs Enter observations during the lab, not from Correct calculations scratch or other paper etc. Results tabulated Complete entries Tables numbered & titled 1. Title and Purpose Sample calculations Analytical method given Correct sig. figs. Analyte given Graphs plotted correctly Sample description Figures & Graphs numbered, captioned & keyed 2. Experimental Plan Graph axes correctly labeled Co-ordinate scale optimized Summary of procedure Co-ordinate orientation Procedure source cited Procedure complete and clear 5. Discussion/Conclusion Numbered Procedure steps Compare precision & accuracy 3. Procedure and Data Discuss Sources of error Reagents ID- grade, brand, etc. D. Erroneous entries Reagent soln ID-conc., initials, date Lined out, not obscured Instrument ID , Make, model, ID no. Include short explanation Omitted sections, pages x’ed

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 8 Attachment C ANALYTICAL CHEMISTRY STANDARDS (Objectives ) http://www.chemistry.org/portal/a/c/s/1/acsdisplay.html?DOC=education%5Ccpt%5Cts_anlchem.html ANALYTICAL CHEMISTRY

(Prepared with the assistance of the ACS Division of Analytical Chemistry)

NOTE: The following supplement is a description of a complete program of instruction in undergraduate analytical chemistry. It is to be recognized that most curricula will not cover all of the areas listed. The supplement should be used as a guide to select topics most suited to a given institution.

A sequence of courses that includes modern quantitative analytical chemistry and instrumental analysis at the undergraduate level should present an integrated view of the theories, chemical methods, and instrumental techniques for solving a variety of real problems in chemical analysis. Students should receive a coherent and progressive treatment of the various aspects of problem definition, selection of analytical method, experimental design, and data collection and evaluation. The problem-oriented role of chemical analysis should be emphasized throughout the student's experience.

The student should emerge from an undergraduate program of studies in analytical chemistry with the following competencies:

 Understand the distinction between qualitative and quantitative goals of determinations  Understand comparison and critical selection of methods for elemental and molecular analyses  Knowledge of sampling methods for all states of matter  Understand statistical methods for evaluating and interpreting data  Understand concepts of validation of data and experimental design  Understand sources of error in chemical and instrumental analysis  Understand interferences in chemical and instrumental analysis  Understand theory and operational principles of analytical instruments including electronic components  Exposure to computer-based data acquisition systems for analytical instruments  Understand the concept of instrument calibration  Fundamental understanding of the principles of and instrumentation for atomic, molecular, and mass spectrometry, magnetic resonance spectrometry, chromatography and other methods of separation, electroanalytical methods, and thermal methods  Understand basic concepts of stoichiometry and basic chemical reactions involving analytes and ordinary reagents  Understand the importance to quantitation of equilibrium and kinetic aspects of chemistry  Understand concepts of availability and evaluation of analytical standards  Understand standardization methodology

Individual topics in analytical chemistry should be presented in the framework of a systematic approach which emphasizes functional roles, facilitates comparison of performance characteristics, and provides a pattern the student can use to understand related topics not included in the formal course work. The courses should include discussion of approaches to optimize performance characteristics such as selectivity, sensitivity, uncertainty, and limit of detection. Examples should be drawn from modern biological materials and environmental chemistry. Some topics in modern analytical chemistry may not require a thorough background in calculus-based physics and/or certain areas of physical chemistry. However, more advanced topics in quantitative analysis theory and instrumental analysis should require these prerequisites.

CHEM 302 QUANT LAB SYLLABUS Spring 2010 4/8/2018 pg 9