CHEMISTRY 3432, ANALYTICAL CHEMISTRY, FALL 2013 Text: Quantitative Chemical Analysis; Daniel C Harris; 8th edition; W. H.

Freeman and Company; 2010. ISBN 1-4292-1815-0. Also available on-line. I recommend, but do not require that you use the latest edition. You may also be interested in a free online/downloadable textbook at: http://web.me.com/dtharvey1213/Analytical_Chemistry_2.0/Welcome.html (click on Analytical Chemistry 2.0 Text files). It will take some time to down load. Michelle Bushey, 115 Oakmont, Rm 203, office: 999-7318, cell: 210-577-9723 (before 10:00 PM) email: mbushey@trinity.edu I am available most M, T, and F afternoons. You might be able to find me on M and F mornings before or after class. I am normally on campus between 8:30 and 5:00. I will not be available on Wednesdays (all day) or Tuesday and Thursday mornings. Since my office door is usually open, I do not keep formal office hours. Charlisa Daniels, 115 Oakmont, Rm 202, office: 999-7842. Lab: MMS 220, 999-7307. Email: cdaniels@trinity.edu If you have any difficulty in finding us, please let us know. We are happy to make appointments. class times: MWF 9:30, CSI 441. Lab W 1:30-5:00, CSI 242 and other locations as needed. Course Summary: This course will cover the basic principles of chemical analysis. We will examine all aspects of chemical analysis so that when you report on the copper content of a soil sample you have a full understanding of what that number does and does not mean. You should come away from this course with an appreciation for the care and planning that is necessary to obtain a quantitative analysis in the chemistry lab. We will examine sampling considerations, matrix influences, experimental design, sample preparation, statistical treatment of data, and finally, the experimental methods themselves. Since it is necessary to rotate groups through the various experiments, you will find that sometimes you perform an experiment prior to the class discussion, and vice verse. Sometimes a lecture topic will not be explored in the lab and a lab topic will not be discussed in the lecture. You should expect this to be the case as it is through the combination of lecture and lab that you will gain in experience and understanding of analytical chemistry. Attendance: This is a four credit hour course with one hour for lab work and three hours for class work. Lab will begin at 1:30 on Wednesday. Some of the labs will run for more than three hours, some less. However, as individuals, you will not write a lab report every week. Although attendance at course lectures is not explicitly required, we expect you to attend the lectures. We realize that situations may arise during the semester that can cause you to miss an occasional lecture. We do not expect this to occur on a regular basis. If you miss a lecture, it is your responsibility to obtain any pertinent class notes, or to make arrangements to complete any missed course requirements. If you begin to accumulate unexcused absences, that may be reflected in the subjective portion of your class participation grade. Also, although we would prefer that everyone arrive at class on time, we would prefer that you come to class late rather than not at all.

Attendance at labs is required. It is generally not possible to make-up missed labs. Possible exceptions to this must be negotiated with me as early as possible in the semester. Illnesses will be accommodated as needed. Grading: three semester exams 33% lab reports (9 total, ICP counts double) 30% (30% on notebooks, 70% on reports) library assignment (topic due 10/7, report due 11/14) 9% subjective-class participation 8% final exam Wed., Dec. 18th, 12:00 noon 20% Note that while specific lecture dates and topics may change, exam dates will not change unless the entire class and instructor reach consensus. Problems are assigned from the textbook. These assignments will not be collected and will not be graded. A solutions manual is on two hour reserve in the library. It is your responsibility to do these problems in a timely manner. At least one problem from these assignments will appear on each semester exam and some other exam problems will be based on these assignments. It is to your advantage to do the assigned problems. We are happy to schedule problem/help sessions if requested. We expect that you will abide by the Trinity Academic Honor Code. You can find it at: http://www.trinity.edu/departments/academic_affairs/honor_code/index.htm If you have any questions how these policies apply to this course, especially regarding the nature of group work, please do not hesitate to ask for clarification. How you approach academic honor says a lot about you as a person. Please note that this course involves a substantial amount of group work. Most of the group work has specifically assigned tasks. We expect that you will follow those assignments. Also, Please note that we will provide keyed copies of exams from fall 2012 for you to use as you prepare for exams this semester. Used of copies of exams from other years will be considered a violation of the honor code. Laboratory: There are nine experiments scheduled for this lab. Most experiments are scheduled for one afternoon. One is scheduled for two weeks. While some of these labs may run a little long, it is possible to complete them in one afternoon, if you come to lab prepared. If you come to lab unprepared, and cannot finish a lab within the given time frame because you are unprepared, you may not be able to complete the lab outside of the scheduled time frame. This laboratory is designed around a team concept. This type of organization mimics what is often found in industry. While it may be several years, if ever, before you enter the chemical industry, working in a team setting forces you to work and interact with other people, a valuable skill. Furthermore, most of these labs could not be completed by one person in the given time-frame. If we did not work with a group system, the labs you could perform would be much more limited in scope and consequently, much less interesting. Although during much of your time here at Trinity you have worked individually on your chemistry, rarely do chemists work alone. Even when you have worked with partners, you have often been on your own to devise ways of sharing the work. In the work place, each of you is more likely to have an assigned task. Thus, each team member will have specific assigned duties for each experiment. Some of these assignments will entail work before the scheduled lab, some will entail work after the scheduled lab. All team members are required to be present when an experiment is performed. If a team member is not present for a particular experiment, that person will not receive credit for that lab. Teams will be rotated half way through the semester. Should a team member prove to be repeatedly unreliable, and repeatedly fail to live up to group expectations and norms, the Manager has the right to fire the group member. The remaining group 2

members will then be expected to carry out the duties of this person. The dismissed group member must then make arrangements to complete the course requirements. Managers and groups are encouraged to respond and rectify potential problems at their earliest appearance. Reports: Only one report will be turned in for each experiment for each group. All team members receive the same report grade. Each team member will turn in yellow pages or notebook photocopies for each experiment. These grades may vary among team members. The notebook grade will comprise 30% of the individual grade for each experiment. All team members must be present when the experiment is actually run in order to provide all components of information input into the experiment. Intra-team communication is extremely important. At the conclusion of the experiment, all team members should be thoroughly familiar with all aspects of the experiment. All team members are responsible for informing all other team members about their individual roles. It is also necessary for all team members to keep proper laboratory notebooks. Each team member should sign the report and keep a personal copy. Each team member is expected to be knowledgeable about the report contents. Notebooks may be periodically inspected. Each experiment should be repeatable from the information in any one of the notebooks. The use of loose bits of paper or use of non-labbook notebooks to record any lab information is not allowed and may result in decreased notebook grades. In addition to the report itself, for each experiment the Manager must submit an evaluation of each team members contribution to the final result. This evaluation must be initialed by the team member in question signifying that they have had the opportunity to read the evaluation. These can be very short evaluations. In addition, each team member, including the Manager, is assigned a contribution percentage, typically 100%. If a team member does not live up to the group expectations, then their percentage should be reported as less than 100%. However, this means that someone took up the slack and someone elses percentage should then be reported as more than 100%. The total for each group must be 100 x # of group members. This percentage will be multiplied by the assigned grade to determine individual grades. This gives you some control over team members whom do not contribute sufficiently to the work. It also gives you a way to reward team members who do more than their share of the work. If you feel that it is unfair for all team members to receive the same grade on a report, this is the way you can change those grades. Typically percentages in the range of 85-115% are sufficient to account for variations in contributions, but this is entirely up to the groups. At the end of the course, each of you will be asked to write a short evaluation of each person you have worked with during the semester. You will also write a short self-evaluation. While not every analysis is perfect, the following are a few errors which can substantially lower laboratory grades: failure to properly specify the time and date of critical records; willful misrepresentation of data; loss or corruption of electronic data or irreplaceable hard copy data; statistically bad results; poor graphical presentation of data; blunders; use of scrap paper in place of notebooks; inappropriate use of balances, weighing paper, glassware, etc., failure to clean up the work area or glassware at the conclusion of the experiment. If the lab is left unclean, deductions may be made on lab reports for all teams in lab on that day. Each report should include: * a title, experiment date(s), the Managers evaluations of each group member and percentage contributions for each group member. Each group member must sign this page. *an abstract. Do not make this section too long! The most appropriate style is that of the abstracts found in Analytical Chemistry. We suggest that you read up to ten abstracts in that journal to get a feel for the style. It is appropriate to summarize the results in the abstract. The abstract should begin with a brief statement of purpose. This is followed by describing, in broad terms how you 3

achieved that purpose. Some specifics on methods/procedures can follow. Summarize with a brief description of the results, including any important numbers. *an introduction. This is a brief section. An introduction should be referenced. We do not want a history of GC-MS. Rather, tell us about what YOU did in lab, and reference relevant material, such as sampling methods used for GC-MS of arson materials. This section is especially useful for labs where you have some responsibility for designing the experiments. *an experimental section with details on solution preparation and experimental design sufficient so as to allow duplication of the experiment by someone of similar experience. This includes details such as type of glassware (volumetric?). Do not simply refer to the handout, but any deviation from the handout should be clearly noted. Any blunder, etc. should be clearly noted. Brief mention should be made of which team member performed which duties so that if necessary, we can refer to the appropriate notebooks. The general format should be that of the experimental sections of articles in Analytical Chemistry. *data presentation, including any calculation, tables, graphs, or printouts. Make sure all data items are properly labeled. Graphs should be presented in a manner suitable to support the conclusions with the appropriate labels and units. Raw data can be included in an appendix, but it is better to imbed important data throughout the report. Label all raw data, and present it in an easily readable form. *data analysis and concluding comments, references to literature data. Include a reference section. I always look for appropriate references. Your textbook, and my handouts can be used but do not suffice. * brief mention of possible sources of error and how they affect results if appropriate. You are only to list likely sources of error, not all possible sources. *any additional items required and specified in individual experiments. The entire report, excluding figures, tables, and raw data, should not exceed six pages and can probably be adequately presented in less for most cases. Course updates, including those related to the lab will be posted on TLearn. You are encouraged to check for updates before beginning any lab. Notebooks: Your ability to keep an accurate and complete record is the measure of your research capabilities. All members of the research team are required to maintain their research notebook up-to-date according to the general guidelines outlined here. All work is dated with the date of the work evident on each page of the notebook, usually on the top of the page or in the left hand margin. A separate page should be reserved for each experiment that you perform, even when you are performing a series of experiments on one day. Each experiment should be given a brief title which may be as simple as Determination of Metal Levels in Soil Samples. The same title should be listed in the index. Reserve the first two pages of your notebook for the index. You are required to keep the index up-to-date. Your notebook should be the type with carbon pages. Copies of all notebook pages from each team member must accompany each report. Carbon pages or photocopies are acceptable. The format for each experiment is as follows: *After listing the title, a brief experimental purpose should be given. If appropriate, a chemical equation should be provided. 4

*A table of reagents should be provided, clearly listing the chemical name, structure, source, amount actually used, number of moles actually used, and accurate descriptions of the measuring devices used. *An exact description of the lab activities, in sufficient detail so as to allow another person to exactly follow your procedures without the lab handout. Observations, detailed methods, etc. should be included in this section. Think of this section in particular as a diary of your laboratory experience. Since you will be divided into teams in this course it is extremely important, that any team members notebook be sufficient to duplicate the experiment. You will need to be explicitly clear as to which information is simply obtained from another group members notebook and which information is original to your notebook. It is important that no data be missing from anyones notebook. Equipment settings, model numbers, etc. should be included. *Analysis of the data (including clearly outlined calculations) follows as well as interpretation of the results. Everyones notebook should contain this section. No notebook will be considered complete without an analysis of the data. Excel printouts can be taped to notebook pages. Notebook conclusions to not need to match report conclusions. *Comments regarding suggestions for future changes in the lab are always welcome. Each notebook page should have the legible name and the signature of the notebook owner. No more than one line should be skipped in a notebook at any time unless a single line is drawn through the extra lines clearly indicating the intention to keep those lines blank. The notebook must be legible to another person. The notebook should also be used for scratchwork, etc. as long as these sections are clearly identified. Mistakes, etc. can only be indicated by a single line through the offending material; no erasures or white-outs are allowed. Treat your notebook as a diary of your lab activities. Assigned duties: Team Manager. The manager is the person in charge. The manager is responsible for the successful and timely completion of the experiment. The manager may delegate duties to other team members. The manager writes the report and thus may have more post-lab responsibilities than other team members. The manager is responsible for ensuring that any prelab planning is completed prior to the scheduled lab time and thus may have more pre-lab responsibilities than other team members. The manager is also responsible for evaluating the contribution of the team members. A brief evaluation of each team member should appear on the cover page of each report. The signature of each team member next to these evaluations ensures that the team members have seen the evaluation and also indicates that they have read and understand the final report. Typically, reports are due 2 weeks following the scheduled lab at 9:30 for each particular experiment (see the lab schedule for details). This should be plenty of time to make sure that all group members have sufficient opportunity to edit reports. Late reports will be penalized 10% per day or part of a day. Under special circumstances, extensions may be granted if sufficient notice is given and the situation is discussed well in advance. It is the managers responsibility to provide draft copies of reports to the other group members in time for revisions to be made. Solutions. The solutions person is responsible for ensuring that all reagents, materials, standards, and solutions are prepared and available for the experiment and/or all calculations regarding solution preparation are done in advance. This assignment may entail more pre-lab duties than other positions. The solutions person should plan out what solutions need to be made and how. Actually making the solutions can be assigned to any team member. Technician. This technician is the person who actually performs the experiment and operates the instruments. The technician needs to become familiar with the equipment prior to the scheduled experiment time, and thus may have more pre-lab responsibilities than other team members. I am available to meet with technician on an appointment basis to discuss the operation of specific 5

instrumentation. The technician is responsible for putting the data into a format that can be easily interpreted by the Manager. Note that the work load of these positions will vary from experiment to experiment, thus, managers should feel free to redistribute duties as deemed necessary. Keep in mind that the responsibility for duties cannot be redistributed, only the execution of the duties. While the Manager is responsible for writing the report, other team members have a responsibility to the report as well. Team members must provide the Manager with the raw data and data interpretation. All team members are responsible for data interpretation. You might find it more expedient for other team members to write sections of the report and then have the Manager assemble the final document. Assembling of the final report is the one duty that cannot be redistributed. All team members are expected to be thoroughly familiar with the report contents. Because of staggered experiment scheduling, no graded reports will be handed back until all teams have completed each particular experiment. However, groups are encouraged to schedule office time to discuss and review graded reports throughout the semester. Also, in order to be sure that each report on all labs is graded consistently, grades on individual labs may be altered as more are graded. You will be informed of any grade changes. Class schedule date topic Section I: What do we want to accomplish? Designing and interpreting an analysis. Course Introduction Analytical Chemistry is what Analytical Chemists Do C. N. Reilley Review of Units and conversions Tools of the trade Prudent Lab Practices: Analytical Approaches and the Proper Use of Glassware Labor Day Understanding and Describing Error Nobodys Perfect The Bell Curve reading

W, 8/28

Ch. 0 Syllabus Ch. 1 Ch. 2

F, 8/30

M, 9/2 W, 9/4 F, 9/6 M, 9/9 W, 9/11 F, 9/13 M, 9/16

Newpaper Ch. 3 Ch. 4

MB and CD at fall ACS. Work on problems together or plan labs. Populations. Dealing with Multiple Data Sets Calibration, Standardizations Sampling: Where from, How much, How many? Isolating the analyte Ch. 4 Ch. 5 Ch. 27 (28 in 7th)

W, 9/18 Simplex Optimization or Mountain Climbing Harvey Ch. 14 Found at (entire text): http://www.asdlib.org/onlineArticles/ecourseware/Analytical%20Chemistry%202.0/Text_Files.html Or Ch. 14 only on TLEARN. 6

F, 9/20 M, 9/23 W, 9/25 F, 9/27 M, 9/30 W, 10/2 F, 10/4 M, 10/7 W, 10/9 F, 10/11 M, 10/14 W, 10/16 F, 10/18 M, 10/21

Factoral Design or Mapping the Mountain finish optimization and design Catch up? More review? Or get ahead! EXAM I Section II Chemical Equilibrium/Acids and Bases Equilibrium, Acids/Bases Strong acids and bases Weak acids and bases More on equilibrium, buffers The Big Lie (activity) polyprotics and extended and complex equilibria Titrations review? Fall Break Titrations cont. Section III Separations and Electrochemistry for Analysis and Analyte Isolation/Selectivity

Harvey Ch. 14

All previous Ch!

Ch. 6 Ch. 8 (9 in 7th) Ch. 8 Ch. 8 Ch. 7 (8 in 7th) Ch. 9 (10 in 7th) Ch. 10 (11 in 7th) Po and Senoza Article

W, 10/23

Electrochemistry Section III Separations and Electrochemistry for Analysis and Analyte Isolation/Selectivity

Ch. 13 (14 in 7th)

F, 10/25 M, 10/28 W, 10/30 F, 11/1 M, 11/4 W, 11/6 F, 11/8

Electrochemistry review

Ch. 13 (14 in 7th)

EXAM II: During Lab timeMaterial from section II only! Potentiometry Potentiometry Voltammetry methods Voltammetry methods 7 Ch. 14 (15 in 7th) Ch. 14 Ch. 16 (17 in 7th) Ch. 16

M, 11/11

Separations, Theory, 1 analyte

Ch. 22 (23 in 7th) Ch. 22 Ch. 23 (24 in 7th), Ch. 24 (25 in 7th) Ch. 24 (25 in 7th), Ch. 25 (26 in 7th)

W, 11/13 (MB OOT) Separations, Theory, 2 analytes F, 11/15 (MB OOT) GC, LC M, 11/18 W, 11/20 F, 11/22 M, 11/25 LC, other separations problem session EXAM III Section IV- Spectroscopic methods of analysis Spectroscopy--- and UV-VIS Instrumentation No classes, Thanksgiving Thanksgiving UV-VIS applications/methods Fluorescence/phosphorescence AA/ICP XRF, wrap up, evaluations FINAL EXAM, 12:00 PM (cumulative!!) Due Dates

Ch. 17 (18 in 7th) Ch. 19 (20 in 7th)

W, 11/27 F, 11/29 M, 12/2 W, 12/4 F, 12/6 M, 12/9 Wed. 12/18

Ch. 20 (21 in 7th)

experiment schedule: Wednesday date groups 1 2 8/28 ----lab lecture for groups 1 and 2 9/4 pKa water 9/11 water pKa 9/18 ICP prep GC/MS 9/25 ICP ICP prep 10/2 GC/MS ICP 10/9 ---lab lecture for groups 3 and 4 10/16 10/23 10/30 11/6 11/13 11/20 11/27 12/4 3 4 XRF XRF CE SEM ----no lab-- EXAM II, during lab time SEM CE LC echem Echem LC --------Thanksgiving week, no lab make up week for misbehaved equipment 8

9/18 9/25 Gp 1: 10/11, Gp. 2:10/2 Gp 2: 10/18 Gp 1: 10/16

11/1 11/6 11/20 12/4 12/9 TBD

*Labs are generally due two weeks after the completion of the lab but there are exceptions. Check due dates at the start of the semester. You will collect a soil sample for subsequent analysis on the ICP. At least the week prior to the ICP experiment the sample must be dried. The sample must be dried at 30C for at least 48 hours. Additional drying time will not harm the sample. A water must also be collected. Use the plastic bottles available in lab, label them and store your samples in the refrigerator until needed. Exam II typically takes longer than one class period to complete. There is no lab scheduled on this day so extra time can be devoted to the exam. The exam will begin at 1:30 PM. Note that all lab reports must be received by Friday, 12/9 by noon. No labs will be accepted after this time unless extensions have been approved WELL in advance. We want to receive the best lab reports possible from you so we are willing to give extensions if that is discussed well in advance and you provide good reasons why an extension will improve the report. We are less willing to give extensions at the last minute because you have made the lab report a low priority. Plan ahead.