1.4: Assignment Details

Pre-Lab Assignments

To prepare for lab, you should do the following:

Wear Protective Clothing: As always, please dress appropriately for a laboratory environment. You must wear close-toes shoes and clothing must cover your body from your upper arms to your knees. You should also have your own pair of protective eyewear, bring them to lab, and wear them the entire time you are in lab. Safety eye wear can be purchased from the Graduate Chemistry Council (GCC). If lab attire is not jiving with your wardrobe, please purchase a lab coat and bring it with you so that you can cover up in lab. No student should be in lab without wearing protective eyewear and appropriate protective clothing.

Prepare by completing the Pre-Lab Assignment: It is absolutely essential that each student be prepared for lab meetings by reading the appropriate module in this manual, and completing the specified pre-laboratory assignments. The pre-laboratory assignments are designed to prepare you to operate efficiently and safely during the experimental module.  You will not be allowed to conduct experiments if the pre-lab assignment is not completed before your lab meeting. If there is an extenuating circumstance that prevents your preparation, please inform your instructors as soon as possible.

The pre-lab assignment must be submitted as a single pdf document on Canvas at least 25 minutes before the scheduled lab meeting. Pre-lab assignments should be typed. If you prefer to write out equations by hand, they should be neat and inserted as an image in the appropriate place (please note that handwritten equations are only accepted for pre-lab assignments and ELNs, but not for reports). If you need advice for how to insert equations or images into your documents, please ask for help at least 48 hours before the assignment is due; an in-person (or zoom) meeting is most appropriate for this issue.

Late pre-laboratory work will not be accepted and will receive a score of zero. Your TA will evaluate the work and return it no later than the beginning of your lab section. Your preparedness will also be evaluated by your answers to oral questions pertaining to the laboratory from the TA and other lab instructors. The pre-lab and preparation accounts for 10 points of each experiment requiring a pre-lab.

For every experimental module there is a general pre-lab assignment and a specific pre-lab assignment.

General Pre-Lab Assignment (same for all modules)

Write a brief introduction to the experiment and the experimental plan using the following outline:

1. Experiment Introduction: In your own words, briefly describe the underlying theory and explain the principle upon which the experiment is based. Keep it concise; lengthy discussions or derivations of equations are unnecessary.
   1. Background (importance/relevance): A brief description and justification of the importance of the topic, with references to source material. What is the topic and why is it interesting and important? This is meant to "hook" the reader so they want to read about the topic.
   2. Theory: A concise paragraph or more describing the general theory for the method/technique used; this section should contain a reference to the appropriate pages of the textbook, or other source material from the literature.
   3. Goals/Purpose: Brief statement of purpose, which should indicate what is analyzed and the technique used. Limit to three to five sentences.
2. Experimental Plan: a short summary of the specific things that you would need to know in order to do the experiment without having access to your lab manual, with the understanding that you will always have a TA available to teach you how to use the instrument. The best way to approach this task is to thoroughly read the procedure for the experiment. While reading, take notes on the specifics of the work. What chemicals will you use? If you have to make solutions, what solutions do you need to make and of what concentration? How will you prepare them? What instrument will you use, and what specific instrument settings will you need to input (sometimes you will find this information in the Appendices that discuss the use of the instruments)? How many runs of each sample will you do; and over what wavelength, or temperature, etc. range? You do not need to write down how to use the instrument; we will teach you that. Bottom Line: we want you to write down only that pertinent information about samples, sample preparation, instrument and instrument parameters, numbers of runs, and other things, that you will need to know in order to do your work.

Specific Pre-Lab Assignment

Each module has a pre-lab assignment on the first page of the module. In general, each pre-lab assignment requires you read the entire module and write out the specified pre-lab assignments in your notebook before starting that laboratory work.

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Electronic Laboratory Notebooks (ELNs)

Warning: Use cloud storage and backup

As you save your documents and develop systems of organizing your academic life, please learn to use a cloud server to automatically save and back up your work. Duke University supports cloud storage through Box and Microsoft tools. Google tools are also a free option. Proper use of these tools is expected. Please ask Dr. Haas if you need some instruction or recommendations for using these cloud-based tools to avoid loosing your work if/when computer hardware is lost or fails.

While we are aware that there are limited computer labs on campus, you also have access to computers also in the P-chem labs. Please plan to always complete your work 48 hours in advance so that any issues with your personal devices do not interfere with timely submission of assignments.

You will complete each experiment as a group, and there will be a dedicated instructor to answer questions. You will record observations using an electronic laboratory notebook (ELN); an example ELN template will be provided for each experimental module. The ELN will contain a written record of your group's activities during lab. Each student should collect a copy of the group data immediately after the lab meeting. Every P-chem lab computer has internet access, and you may either email data to yourself, save it using OneDrive, Google Drive, or Box, or collect it using a usb drive.

You will make the ELN your own by filling in your own work in the Background, Theory, and Purpose statements (from the pre-lab assignment). Edit these statements as necessary using the pre-lab assignment feedback from your instructor. The data collection should be done in your group. Then, do your own work to complete the questions and data analysis in the ELN. Your completed ELN must be submitted for grading before the end of the lab meeting. Extemtions may be given if extra time is needed to complete the data anaysis outside of the laboratory meeting. The maximum extension is up to the next scheduled meeting (~1 week). The pre-lab assignment accounts for 10 points, and the ELN accounts for 30 points for each experimental module.

Using the electronic laboratory notebook (ELN) template

Templates for each ELN will be provided as a guide to help you understand the minimum expectation for what should be recorded during the laboratory session. You should record all additional information and observations that you think is relevant. One member of the group should create a shared version of the ELN that will be used during the laboratory period, and in which all group members can contribute to the Observations and Data section. Then, each group member should make their own copy and complete the individual sections with their own work. To guard against the possibility of plagiarism, do not share an electronic copy of any ELN that contains your own work.

There are three sections to each ELN: The "Observations and Data" section should be edited during lab while your group is working together. The other sections must be written by you and should be your own work.

Note

Before beginning any electronic laboratory notebook entry, track your changes. This way if you accidentally erase good data it can be retrieved afterwards. SAVE OFTEN when working outside the safety net of cloud-based autosave and backup.

• In Microsoft Word, select Highlight Changes from the Track Changes option under the Tools menu.
• In Google Docs, revision history is automatically saved as long as you are connected to the internet.

Pre-Lab section:

(Your own work) This is where you will copy/paste your own pre-lab work.

Observations and Data (Group data collection):

Record all observations and primary data as a group. This should include the actual procedure, instrument used, instrument tolerance (error), instrument settings, any notable observations, and all data collected during the lab period.

This section, in which you will have the same information as the rest of your group members, should contain only the information collected while in the laboratory. It should not contain your evaluation the data/observations in any way (that is the post-experiment work). If data are being collected by hand (handwritten on paper) it should be in clear, easy to read format. This handwritten data should be immediately entered into a shared ELN file. For data that are collected by a computer interface to your equipment, note the specific name of the data file in case you have to retrieve the file later! Take screen shots as necessary to capture important data to insert into the ELN. Write observations for each run, including "bad" or aborted runs, in a narrative style and state where the actual data file can be found (including filename) when needed.

Post-Experiment work:

(your own work)

Calculations of results and uncertainties: Unless otherwise instructed all calculations of results and uncertainties should be included as part of the laboratory notebook. In this course doing so will require the typing of a lot of mathematics. Please remember that you always have the option of writing your calculations out neatly on plain paper and scanning it to make a digital image that can be incorporated into an electronic notebook entry. Mathpix is recommended to help you convert equation images to Latex for insertion into typed documents (use the Free & Educational use option!).

Discussion of results: In this section you truly “think in the notebook”. Reflect on what you have done. Write this section in your own words after the observations are completed. Include charts, graphs (see below), tables or rearranged data and your rambling thoughts. Remember this is not a formal report. You want to be neat and complete, not necessarily a literary star. This section need not be long, but it should contain all pertinent information.

Graphs: Often you will generate graphs from your primary data files. They must be represented in this section of the laboratory notebook. It is not difficult to include digital copies of graphs within the electronic laboratory notebook, but you should remember that such images can easily make the file sizes large and thus difficult to work with. Below is a procedure that will work to include copies of your graphs in the notebook while minimizing the overall size of the resulting file. A reliable way to capture graphs/plots to insert into your lab notebook is to use WinSnap for PC (or screenshot on Mac). Each lab computer has WinSnap installed. You can take a screen shot by pressing SHIFT + COMMAND + S on the keyboard. This will allow you to select a region for capture and the image will be saved to the clipboard. Press CONTROL + V to paste. You can also open the WinSnap program from the desktop shortcut instead of using keyboard shortcuts. (SAVE OFTEN!)

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Reports

In this course, ELN's that include answers to discussion questions (post-lab questions) are considered "reports" of your work.