CHEM 3111L

Laboratory Calculations and Accuracy Policy

Fall 2011 Scope and Goals. This policy applies only to the six numbered experimentsnot to the exercises or to the special projects. Calculations and accuracy will be graded separately. To prevent inadvertent calculation errors from affecting your accuracy grade, we will check accuracy directly from your raw data. As described in the experiment handouts, up to 35% of your grade for each experiment will depend on your calculations, and up to 40% on accuracy. Our goal is for you to master these important skillsnot to penalize you too harshly for mistakes. Therefore, this policy gives you opportunities to build mastery by correcting your work and resubmitting it for partial credit. Sample Calculations. Each experimental procedure will include sample problems just like the calculations you must perform to determine your analytical results. Answers will be given. You must demonstrate that you can obtain exactly the same numbers by writing out your solutions to these problems in your laboratory notebook. Clearly show all work with proper units and labels throughout and follow the rules for significant figures, guard digits, and rounding described in the Significant Figures handout. Sample calculations do not have to be done before you start the experiment (although this is strongly recommended), but they must be attached to your lab report with the rest of your carbonless notebook pages. If you forget to submit sample calculations or if what you submit is not completely correct, you will (initially) receive a zero for the calculations portion of your report grade. Sample calculations will not ordinarily include uncertainty propagation. The handouts for each experiment will explain how to calculate the required uncertainties. Raw Data Submission. We will use our own grading spreadsheets to check your accuracy directly from your raw data. To facilitate this, you must submit your raw data through Moodle, using the data submission spreadsheet template that we will provide for each experiment. Carefully enter your data in this spreadsheet and verify that it exactly matches the data in your notebook. Do not enter data from any trial that you rejected as a statistical outlier (using a Grubbs test) or because of a known lapse in experimental technique. Before uploading, rename your file as in the following example, appending an underscore followed by your own surname and one or more initials: Exp1data_CooperBT.xls (or .xlsx) This file should not contain any calculationsonly raw data, entered in the designated spaces. It must be an Excel file; if you use a different spreadsheet program you must be able to open the Excel file we provide and save it in native Excel format. Your report is not considered to be submitted (and thus subject to the late report policy) until your raw data has also been uploaded to Moodle. And you can expect up to a 10% deduction from your report grade if your raw data is not entered and submitted correctly, so please follow these instructions carefully. Calculations Spreadsheet. Unlike the sample calculations (which must be written out by hand as described above), you are required to use a spreadsheet to perform all calculations for your unknown, including uncertainties. Your calculations spreadsheet must be a separate file and must also be uploaded through Moodle, named (in parallel to your data submission spreadsheet) like the following example: Exp1calcs_CooperBT.xls (or .xlsx) This spreadsheet may be organized however you like, but we recommend starting with a renamed copy of your data submission template, and we ask you to be conscientious about marking all quantities with units and labels. To help us find your calculated results (any

2 numbers reported in your abstract, including uncertainties), please highlight them by formatting them in a bright color or in boldface. And please do not round or limit the number of digits displayed for calculated quantities; use the general cell format whenever possible. We strongly recommend testing your spreadsheet with the data from the sample calculations. You will know have done something wrong if your spreadsheet does not give the correct answers from this data. (Unfortunately, you will not be able to test statistical or uncertainty calculations this way.) Your instructor will be happy to help you troubleshoot your calculations spreadsheet if you are struggling with this. Calculations Grade. As with the raw data, your report is not considered to be submitted until your calculations spreadsheet has been uploaded to Moodle. Note also that it is not acceptable to perform calculations externally and simply enter the results in your spreadsheet. You may certainly check them manually, but all calculations must be done using spreadsheet formulas, starting from raw data. It is much easier to fix mistakes this way and (once you become comfortable with spreadsheets) to prevent making mistakes in the first place. However, we will not grade the spreadsheet itselfat least not initially. Instead, we will compare any intermediate and final results from the data tables in your report to values we calculate from your raw data using our own grading spreadsheet. We will also compare your reported uncertaintiesalways as 95% confidence intervals. If all of your results are correct, you will receive full credit. But if any of your reported numbers disagree with ours, you will (initially) receive a zero for the calculations portion of your report grade, and you will be asked to resubmit your calculations according to the procedure described below. Recalculation Submission Protocol. Calculation errors should be unlikely if you follow our recommendations. But if you nevertheless receive an initial zero for calculations, you will be expected to resubmit your calculations for partial credit. The actual point penalty will vary with the severity of the mistake: mere typographic errors will be penalized the least, while outright omissions will be penalized the most. Recall that we check your calculations by looking only at your reported results. Therefore, if we return your report for recalculation, we will indicate what results are incorrect, but we will not troubleshoot your spreadsheet or tell you where the mistakes were made. Instead, it is your responsibility to find your errors, correct them, and explain what you did. This will require a face-to-face meeting with your lab instructor, according to the following protocol: 1. Save your calculations spreadsheet under a new filename, like this: Exp1recalc_CooperBT.xls (or .xlsx) 2. Once you have found and corrected your errors, email this file to your instructor and arrange an appointment. Be sure to bring your graded report (and if required, your rewritten sample calculations) to this meeting. But do not rewrite the report; there is no re-grade opportunity for the report itself. 3. Your instructor will review your original and resubmitted spreadsheets in your presence, and ask you to explain your mistakes and show how you corrected them. 4. Your instructor will then either assign partial credit on the spot or ask for additional corrections, at his or her discretion. 5. To ensure timely feedback (which is to your benefit for future reports), resubmissions will ordinarily be due within one week after the graded report is returned to you. 6. If your recalculations are late, the pending fraction of your grade will be reduced by 10% per school day, or to zero beyond five school days from the deadline. 7. Your instructor may waive the requirement for a face-to-face meeting if your mistakes were trivial or if you only needed to resubmit the sample calculations.

3 Finally, although we expect you to find your own calculation errors, you are always welcome to ask your instructor for help if you are having trouble with this. Accuracy. We test the accuracy of your measurements using samples with analyte concentrations known only to the instructors. We carefully prepare these samples from high-purity materials, so their concentrations may be viewed as true values (). For each experiment, your instructors will also estimate , the population standard deviation for the measurement. You should think of as the run-to-run variation that can be expected for students with acceptable (but not necessarily excellent) laboratory techniqueas a measure of the intrinsic precision of the experiment. The grading scheme is simple: if your measurement was accurate, you will receive full credit for accuracy. If it was not accurate, you will (initially) receive a zero for the accuracy portion of your report. Accurate and inaccurate are defined according to the following table: Difference from true value within 2 (accurate) between 2 and 3 outside 3 (inaccurate) Accuracy points earned 100% 80% 0%

If we have estimated correctly, the result determined by a student following proper technique will fall within 2 of the true value 95.5% of the time, and within 3 of 99.7% of the time. The corresponding probabilities for falling outside these ranges due to random error are 4.5% and 0.3%. But because we tend to estimate conservatively, the likelihood that you will be judged inaccurate due only to random error is even lower. Therefore, you should view an 80% accuracy score (between 2 and 3) as a warning that you must improve your technique, because you are rather unlikely to have fallen in this range due to random error alone. Invalid Data and Outliers. Accuracy requires vigilance. You must critically evaluate your own laboratory technique at all times during an analytical procedure. It is your responsibility to discard and repeat any replicate measurements that you know to have determinate errors because of spills, air bubbles, dirty glassware, or other lapses in technique. Draw a single line through any invalid data in your notebook, and write a brief justification for its deletion. Never use a data point that you know to be invalid, even if it appears after the fact to fit the rest of your data. This includes scout titrations, which intentionally sacrifice accuracy to obtain a quick estimate of the equivalence volume. An outlier is a replicate for which you are not aware of any determinate errors but that nevertheless appears to differ significantly from your other trials. Outliers may be rejected only by proper application of a Grubbs test, as described in Chapter 4 of Harris. Note that the text does not give a critical value of G for n = 3, because you should always perform a fourth replicate if you suspect an outlier. But if time limitations or other circumstances prevent this, you may use Gtable = 1.153 for n =3 and 95% confidence. We strongly encourage you to calculate your results and test for outliers before you leave the lab. Most students have calculators with built-in statistical functions, and at least one computer will be available in the lab for quick statistical calculations. Although our grading spreadsheets perform outlier detection automatically, we may penalize you if your results were only accurate after we rejected an outlier that you failed to check. Never enter invalid replicates or outliers in your raw data submission spreadsheet. Precision. We do not grade precision directly, but it will be impossible to detect outliers if your overall precision is poor. And although good precision does not guarantee accuracy, it is usually a sign of technical competence. Your instructor can advise you on how precise a given measurement should typically be. If you judge that there is too much scatter in your

4 data, you may elect to repeat the entire analysis (throwing out all previous trials) before submitting your results for a grade. This will not change your report deadline. And since real-world sample quantities are often limited, you may incur a small point deduction if you have run out of sample and need a new one. Repeat Opportunities. If you receive a zero for accuracy on an experiment, you will be allowed to repeat the analysis for partial credit, according to the following protocol: 1. Make arrangements with your instructor for laboratory time. You can usually expect to be allowed to work during one of the other lab sections, and additional make-up sessions may be offered if needed. 2. We will not re-grade entire lab reportsonly your new raw data may be submitted. Do this simply by emailing a new data file to your instructor. Name it like this: Exp1repeat_CooperBT.xls (or .xlsx) 3. You will earn 80% of the original accuracy points if you are within 3 of the true value on your second attempt. Third attempts will not be allowed. 4. One repeat opportunity is guaranteed; repeat opportunities for additional experiments may be granted at the discretion of your instructor if time allows. 5. Deadlines for repeat opportunities are at your instructors discretion, but you are expected to submit your new raw data the same day you finish collecting it. 6. If you do not complete the repeat attempt on the agreed-upon date or if you do not promptly submit your new data, the pending fraction of your grade will be reduced by 10% per school day, or to zero beyond five school days from this date.