A new approach to undergraduate analytical chemistry - American

vinced that for many students such an ex- perience is the most important educa- tional opportunity they participate in as an undergraduate. The intens...
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A New Approach to

UNDERGRADUATE ANALYTICAL CHEMISTRY A group-lea rning M and project-based

any educators have begun to question the methods we use to teach science. They advocate changing our current emphasis on covering a broad spectrum of content to an emphasis on teaching the process of science: how scientists pose questions and seek answers. It is argued that students equipped with strong problem-solving skills will be able to learn the content needed to solve problems they encounter in the future. Having involved significant numbers of undergraduate students in independent student research projects over the past 14 years, I have become convinced that for many students such an experience is the most important educational opportunity they participate in as an undergraduate. The intense involve ment in a project in which they must apply content toward solving problems, and in which there is no detailed road map for how to proceed, demonstrates to undergraduate students how science really works. In 1991, I began to introduce a series of changes aimed at imparting the positive aspects of the research experience into my undergraduate courses in analytical

Thomas J. W e n d Bates Co//ege

approach demonstrates how science really works chemistry. Although these courses now emphasize the process of analytical chem. istry, thereby better serving the needs of the students, little in the way of content has been sacrificed. Previous courses

Prior to 1991,two courses.“Introduction to Analytical Chemistry” and “Instrumental Methods in Analytical Chemistry,” were offered. These were rather traditional courses in quantitative and instrumental analysis (see box on p. 473 A), and the survey nature of the introductory course led to considerable repetition and overlap of material between the two. (For example, although the theory of cbromatography was covered in the introductory course, this material had to be repeated in the advanced course for the presentation of modern chromatographic methods to have much meaning.) One source of dip

470 A Analflical Chemistry, August 1, 1995

satisfactionwith these courses was that the importance of separation methods in chemical analysis was minimized in the introductory course because most texts on quantitative analysis provide only a cursory description of chromatography at the end of the textbook A more important concern than the order and content of the lecture part of the courses was whether the laboratory experiments adequately represented analytical chemistry. Experiments performed in the introductory course were traditional wet methods of analysis, whereas those performed in the advanced course were typ ical experiments in instrumental analysis. In their 1975textbook, Laitinen and Harris (1) defined the analytical procedure as containing five steps: definition of the goal, sampling, separation of the soughtfor constituent from other species present in the sample, measurement of the d e sired substance, and evaluation and interpretation of the data. The laboratory experiments performed in both courses, but especially those in the introductory course, almost uniformly focused on the measurement and data evaluation steps while virtually ignoring the goal-setting, sampling, and separation steps. Unknowns in the introductory course were almost always certified samples obtained from commercial sources. 0003-2700950367-4701\$09000

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The group-learning approach

?he two new c o m s are “Separation Science” and “Analytical Spectroscopy and Elec!rochemisW (seebox on p. 473 A). Although these courses present basically the same material as the previous courses, the way in which some of the material is COYered has been markedly changed to involve a groupleaming approach. Gravimetric analysis is not discussed as a specific method, although many of the featuresare presented in electrochemistry when we cover electrogravimetric methods. ?here is also no section specifically devoted to titrations, because titrations are performed in our ht-year chemistry course and by students in the organic and physical chemistry labs and are also discussed in the classroom units on acid-base chemistry and electrochemistry. A problem with the new format is the lack of a suitable text for an undergraduate course in separation science. Most quantitative analysistexts provide too little coverage of chromatography, and most

instrumental analysis texts do not cover chemical equilibrium in enough detail. I have solved this problem by using a variety of reserve readings in separation science (quantitative analysis books for chemical equilibrium, instrumentalbooks or chapters from physical methods books for chromatography, literature, and review articles) instead of a traditional textbook. For the unit on chemical equilibrium in “SeparationScience,’’which involves a p proximately one-half of the semester, the class is divided into groups of three or four students who work together for the entire unit. Groups are assigned after collecting information on the students during the first day of class, and attempts are made to balance the groups on the basis of background and interest. Upper-class students with the most experience are assigned to different groups, and each group usually has both chemistry and bio chemistry majors. Groups are Usually of mixed gender; although I have never felt

certain that this represents the best a p proach, students, when asked, have consistentlyexpressed a preference for mixedgender groups. Each day the students are given prob lems to work on within their group. My role is that of facilitator,to move among the groups and offer suggestions, without offering actual answers, that get the students thinking in the right direction. If one student in a group recognizes a concept needed to solve a problem, she or he is to explain it to the remainder of the group. When all groups appreciate a concept or solve the problem, I summarize the finding. Homework problems are assigned on a daily basis, and after students attempt them individually, each group meets to discuss the assignment before coming to the next class. The unit on chromatography also serves to demonstrate aspects of the historical d e velopment of science. In this unit, the students must read certain signhicant papers on the development of chromatographyas Ana/yiica/Chemistv,August 1, 1995 4’H A

well as several review articles: these articles are then discussed in class. The most significant change in the courses is in the lab. Instead of weekly ex periments, students now undertake semester-longprojects in groups of two to three. (The lab groups are purposefully differentfrom the grouplearning teams described above.) These longer experiments (see box) also lend themselves to class themes. For example, one year in “Separation Science,”the entire class analyzed differentconstituents of coffee, including volatiles, acid and baseheutral semivolatiles. amino acids, and methyl xanthines. laboratory groups are given only topical information about their project, and the first responsibility of each group is to meet with me and the science reference librarian to conduct a computerized search of Chemical Abstracts. Based on the results of the search, copies of appropriate articles are obtained and the students are responsible for determining what procedure will be used for proper samplingand pretreatment to isolate the analyte of interest from impurities. I discuss aspects of sampling and pretreatment with the students and approve any procedure before they begin. Frequently they must order some chemicals or assemble an apparatus (ex., column chromatography or purge-and-trap device) to complete the pretreatment procedure. During the initial weeks of the course, as the groups are gathering the necessary background literatwe, I work with each group individually to develop an appropriate level of proficiency with their instrument. Once checked out on their instrument, the groups are allowed (and actively encouraged) to work “offhours” in the lab. (‘‘Offhours” constitute any hours other than the afternoon in which the lab is actually scheduled. Students can come in any time I am in the building to perform any activity provided I know that they are in the lab. On evenings and weekends, activitiesare Limited to specified procedures such as running chromatograms and data workup and analyses that I know do not present safety hazards.) During the semester, each student is required to work 30 h in the lab. and group members are encouraged to coordinate activitiesso that they do not spend all that

time together. For example, once a group knows how to prepare the standards, it might make sense for only one member of the group to actually prepare them. Each student logs his or her hours in the lab notebook, annotated to show the tasks that have been done (literature search, reading literature, assembling apparatus for sample workup, learning how to operate the instrument, etc.). Each student writes an individual r e port in the format of an article in Analyfical Chemistry at the end of the semester. The members of the group share the data, but the presentation, interpretation, and discussion of the data in the write-up is done individually. A draft of the Inlmduction and ExperimentalSection is due about three-fourths of the way through the term. 1critique the drafts and meet individually with each student to discuss my comments.

the topics already covered. The most im. portant attribute of group problem solving, however, is the active nature of the learning. Both the students and I gain a clear sense of what each student understands and where each student is confused. The classroom atmosphere is also far more relaxed than when 1lectured to them. A lot of talking is going on, the overwhelming majority of which relates to the problems being covered. The grouplearning environmentalso forces students into the role of teacher. Having to explain a concept to another student is an especially effective way to solidify one’s understanding of the material and provides each student with more outlets for help and advice. The groups do meet off hours to go over problems, as is “required” in the course, and as a result, I find students spending far more time working on prob lems than was done in the past In previous years, it was typical for students to hy a problem on their own, almost immediately get stuck, and then turn in blank answer sheets. Now a group member comes to see me before the problem is due and explains where they as a group decided they are confused; I can then assist them in a meaningfulway and they can continue working on the problem. The implication of such a grouplearning approach is that cooperation, not competition, is the key to success in the course. I make the point to the students that it is best if everyone works together to help each other underThis year we are also byhg a peer restand the concepts presented. new process for the 6rst time in which stuRelying on people to work together in dents will be paired with a partner who is a cooperative manner does run the risk not in their lab group to assess both the that certain groups may be dysfunctional content and writing style of their report and therefore compromise the learning During the last scheduled lab, we hold an process. I spend a substantial part of the “Analytical Symposium” (complete with first class explaining group learning, d e pizza, soda, and ice cream), during which scribing my expectations, and stressing each group gives an oral presentation of my availability to discuss problems should their project to the rest of the class. they arise, and 1hy to monitor the situation so that I can intercede if problems do develop. Although I have not yet had a Pros and cons of the new format group that I would consider dysfunctional, From my perspective, there are many ad1 did have a group that was ignoring my vantages to the new format. The new or- suggestions in class and then not accomder of topics provides less repetition of plishing much. After I talked individually material between the courses and a more with each member of the group and relogical and coherent flow to the topics; the stated my expectations and hopes for extra time is used not to introduce more them, the group was able to turn the situatopics but instead to spend more time on tion around.

4’12 A Analyiiml Chemistry, August 1, 1995

Cooperation, not competition, is the key to success in the group-learning approach.

A more likely occurrence is a group in which one member does not seem to coop erate with the others. In the occasional case where this has occurred, it has involved a bright student who seemed to resent having to share his or her insights with other members of the group. These individuals g e n d y stopped participating in the off-hour sessions, but the remainder of the group had enough members to meet and be productive. When using group learning, it has been tempting to by to ensure that everyone fully understands every concept before gcing on to new material, but unfortunately, one or two students can then slow down the remainder of the class to unacceptable levels. In those cases, I have made a point of encouraging the student(s) having the problems to see me individualiy for additionalhelp. In the two years I have used group learning, however, l have not had a single student to whom the rudimenm concepts of equilibrium seemed beyond reach. All of them are able to start the most complex of problems, and they can usually tell me quite specitically where they are confused. ' At times, especially in the first few weeks, progress can seem slow, and it is therefore important for the instructor to be patient when using group learning.The pace does pick up duringthe second half of the unit on equilibrium, however, because the students have a thorough understanding of the basics and because far more learning now occurs outside of the classroom than previously. I fmd that I can then assign a difficult problem and the students can make reasonable progress on their own. h b t - b . M d labs In the projea-based labs, the students gain a more realistic sense of what it means to undertake a chemical analysis. They a p preciate the necessityof searching the literature and realize that when several methods of analysis are available, they will have to select the one that is '%est" for their needs.They realize how the criteria and demands of the analyst and the particular nature of the sample ultimately i n k ence the choice of the "best" method. They see that the work-up is different from the instrumental measurement and

Comparisonof old and MW courses

"Introduction to Analytical ChemistN"

"Se

Class tom

Labs Determination of pctassium . phthalate air using GC/MS Gravimetric anal is of chloride Determination of trihalomethanes in drinking water using GC/MS Determination of?hloride by titration Determinatlon of nitrate and sulfate in Determination of water hardness rainwater using Ion-exchange Spectrophotometric determination of chromatography wth indirect manganese in steel spectrophotometric detection Analysis of iron by potentiometric titration Detection of the amino acid content of Identification of an amino acid v etables using reversed-phase LC w% fluorescencedetection Determination of caffeine, theobromine and theophylline in chowlate

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"Analytkal Speclroscoov Electrochemistry"

nuorescenc Electrochemical Ion-selective eiect Voltammetric meth-"-

nee of $-naphthol as a function Determinatlon of PAHs charbrmled meats usi nation of chloride, nitrate. and Huorewce detwo Determinamof lead in soil as a function e bv ion-exchanae of distance tmm the mad chromat6graphy Determination of sodium in water by AES Determination of heavy metals in sludges fmm secondaw waste treatment dams Analvsis of aasoline usina GWMS

that both have different sets of questions and demands. The "open lab" format helps eliminate the notion that science occurs in three hour time blocks, and it is typical for the students to spend far more than the re quired 30 h on their project. For exam ple, of 14 students in last year's class, one worked more than 50 h, five more than 40, and only one less than 35. Students have also been willing to work at unusual hours if it would help to enhance their

project For example, one group went out to a roadside at 600 a.m. to obtain an air sample prior to rush hour and compared it to one collected at 900 am. the same day. Another group heard thatrainand lake wzr ter on M t Washington in nearby New Hampshire had unusually high levels of constituentsof acid rain,so they hiked the mountain to obtain samples (although they insisted thatthe time spent hildngwould not count toward the 3Gh laboratory requirement). Ana/ylica/Chemistry, August 1, 1995 473 A

Sampling is an especially enjoyable part of the lab. We have gone to the local supermarket to purchase oysters (which we later blended into an oyster frapg), to Burger King to order six hamburgers without the buns, and to a local candy shop to purchase chocolate (we managed to purchase enough chocolate for sampling of another type). Students sampling with a pump and Tenax trap on the quad have enjoyed explaining what they were doing to inquisitive passersby, and tbe group am alyzing the amino acid content of coffee, which joked of looking for some shred of nutritional value in coffee, found much higher amino acid levels when they brewed their coffeein 6 M hydrochloric acid their sc-xlled strong brew. I believe that enjoying the lab is important, and there is no question that both the students and I have more fun with the project-based labs than we did with the previous experiments.Students can have a good feeling ahout analytical chemishy, without sacrificingthe discipline that is needed to perform reliable analytical measurements. The project approach has also generated a level of independence, critical thought, and empowerment that I did not observe in the previous format. By the end of the semester students are quite willing to work independently and make decisions without verifying them with me. Our instruments are spread throughout several rooms in the chemishy building, and I circulate among the groups monitoring their progress and providing assistance as needed. Prior to the project labs, when I bad groups working on several instruments, the students always seemed to be sitting and waiting for me to arrive because they were unsure of what to do next and unwilling to proceed without my authorization. During the first year I used the project labs I was surprised to enter a room and find that the students had taken apart their recorder. It was malfunctioning, so they had read the manual, diagnosed the problem, and were proceeding to fix it. This degree of iddependence has been typical by the second half of the project labs. Although no group has ever completed its project, because there is not enough time in the semester to perform sufficient replications of unknowns or analyze suf-

ficient numbers of standards to achieve the desired degree of accuracy, all of them have experienced a satismng sense of accomplishment. I have often encountered students in the lab or lounge explaining their projects to other members of the class or to students who are not even in the class. Many tell me how they had a long phone conversationwith their parents describing the particulars of their projecL Because each project incorporatesbasic concepts or techniques that are eventually covered in the lecture part of the courses (usually long after the students are versed on the methods needed for their project), the members of each group

The project approach has generated a level of independence, critical thought, and empowerment not observed in the previous format. experience at least one day in class when they know more about the topic than the others. It is obvious that on those days they feel f i e “experts”on the material, and I make a point of drawing them into the presentation and taking about some of the particulars of their project. All of the groups analyze real samples and do a suffcient number of standards to get reasonable values. They appreciate how difficult and demanding a process it is to get a reliable analytical number when performing trace analysis and realize that procedures that were originally time consuming would become more routine with repetition. The desire to have some results to report to the class in the oral presentation also provides a strong motivation for the students to put in extra time on their project. They appreciate bow much work went into the results they got, and a sense of pride pervades the class during the oral presentations. The impor-

474 A Ana/yiica/ Chemistry, August 1, 1995

tance of working with other members of a group, budgeting their time, preparing a report that takes the format of a journal w ticle, and presenting their work orally all contribute to a “real-world”aspect of the lab. There is no question that the new format, especially in lab, has a different emphasis than the previous one. One major difference in the lab is that students do not get the repetitive work performing experiments that emphasize proper tecbnique and use of glassware, and for which they are graded on the accuracy and pre cision of results. Proper use of glassware is still emphasized, however, in the execution of the projects. Standard solutions are prepared using volumetric glassware, and the trace levels required for the projects necessitate serial dilution.The concept of introducing and propagating error becomes especially apparent to the students as they consider how to prepare trace-level standards. Another difference between the two formats is that students in the projectbased labs do not get the chance to operate every piece of equipment in the department. The trade-off becomes one of the relative value of understanding one instrument in great detail versus many instruments super6ciaUy. Almost all the instruments need some repair during a project, and students experience using the manual for troubleshootingpurposes. I also encourage them to read the manuals when recording data to learn about features that might facilitate the interpretation and presentation of data for their reports or that might make the accumulation of data easier or more automated. Having ma5 tered the operation of one sophisticated instrument, such as a GCIMS, gradient HPLC, or ICP spectrophotometer,the students are not timid about approaching a new instrwnent when required in another course. From other projects, and through the lecture portion of the courses, they appreciate the capabilitiesof other instruments that they have not had the chance to operate. The project-basedlabs use several SD phisticated, and therefore expensive, pieces of equipment, the majority of which were obtained through instructional grants from the National Science Foundation. Costs will be incurred in purchas

THE INDUSTRY ing chemicals and supplies the first year that each project is undertaken, but once this is done, the costs are comparable to, if not less than, the costs associated with purchasing unknowns and primary standards for a quantitative analysis lab or materials and supplies for an instrumental analysis lab. Students occasionally request an item that is too expensive to purchase (we built our own purge-and-trap device rather than buy a commercial model for several thousand dollars), and they then appreciate that budgetary constraints sometimes limit our ability to conduct an experiment. Several students who have participated in the new courses have now gone on to attend graduate school, seek employment in industry, or participate in summer research at Bates or elsewhere. I have yet to hear a single complaint from them about having an inadequate background in analytical chemistry. What I have heard is how much they still remember about their laboratory project and how much they feel it helped them to know what to expect when conducting research or performing chemical analyses. I am convinced that a grouplearning approach is a particularly effectivemethod for teaching quantitative topics such as chemical equilibrium, and would urge any skeptics to try it once. The majority of the equipment used in performingtheseexperimentswas obtained through the Inshctional Laboratory Improve ment Program of the National Science Founda tion (Gradient Liquid Chromatograph, CSI8551126:Gas ChromatographIMassSpectrometer, CS147XfJ27;Inductively Coupled h m a , DIiE9452296). Reference (1) Laitinen, H. 11:Harris. W. E. Chemical

Analysis, 2nd ed.: McGraw-Hill New York, 1975.

Thomasl. Wenzel is Professor of Chemist0 at h t e s College and President-Elect of the Council on Undergraduate Research. He hns taught counes in general and anal*'cal chemistry for the past 14yean, and currently cam'es out research with h e aid of undergraduate students in the areas of NMR shiff reagents, selective solvents for GC, and lanthanide luminescence detection in LC. Address correspondence about this article to him at Department of Chemis. t o , Bates College,5 A n d m Rd., Lewisfon, ME 0424M092.

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AnalyticalChemlstry, August I, 1995 475 A