Chem 181, Advanced General Chemistry Laboratory, Secs. 22A, 23B, Fall 2018.

Lab 7


Lab techniques: vacuum filtration, pH testing.

Lab notes:
This lab is difficult. There are many steps where things can go wrong, and you should read the procedure very closely. Monitoring the pH requires some care because the solution is so strongly pigmented and will need to be diluted. The theoretical aspect of this lab is also non-trivial. Unfortunately, this week seems very packed with midterms for many of you, but please put extra effort into the pre-lab and preparation for this week's lab.

Thought question: Why is keeping track of the pH so important for this lab?

Feedback on various assignments.
Formal report:
This was a hard assignment. Don't be discouraged if you got a bad grade, because others did poorly as well. This assignment is difficult because technical writing is difficult. There are two such assignments left, each worth more points, and you can definitely improve by taking the time to identify what you're doing wrong and fixing it. To this end, I will host additional office hours for the next lab report on Wednesday 11/14 from 5:40 pm to 7:10 pm. Let me know if you want to attend but have schedule conflicts at this time. Bring your first drafts and any questions that you have. The more prepared you are, the more helpful I will be. I plan on going over common mistakes from the first formal report, addressing general questions, and then having you work on an activity where you design a rubric and grade part of each other's report. During this time, I will answer individual questions. Notes for the next formal report. There will be new sections to write (the introduction) and a small addition to one section (procedures and methods). You have gone over the introduction section in lab lecture. In the procedures and methods section, you should not only describe the experimental procedure but also discuss why the procedure works (i.e. what the purpose of all the reagents you're using is). Finally, note that screenshots of spectra are not sufficient for report figures. You need to make your own figures using the data exported from the spectrometer software.

Lab notebook:
Decent, for the most part. Please make sure you have enough observations in general.

Post-lab for WebMO lab:
Unfortunately, this assignment also did not go very well. Presumably this was due to a confluence of factors: (i) midterm the next day, (ii) post-lab rubric this time was quite strange, (iii) MOs are hard. Also, please note that you should be using the post-lab template on Canvas, not LabArchives. Canvas is more up-to-date, and my numbering scheme follows the Canvas questions.
Post-lab for silver nanoprisms:
Nothing major here. Note that the reason nano is such a buzzword is because nanomaterials behave very differently from bulk materials, and we should not expect an "infinitely large nanoprism"---that is, a bulk material---to behave the same way as does a (nanoscale) nanoprism.

Lab 5-6


Lab techniques: micropipette use, venting, UV/vis spectrophotometry, cleanliness.

Lab notes:
(Week 1.) Nanoparticle synthesis requires very clean glassware, so be sure you do not introduce any contaminants into your solution. You will be picking up clean glassware from the stockroom. In addition, the colors of the nanoparticle solutions will be very sensitive to the volumes of reagents measured out, so take care with that also. Follow the Experimental Information section of the LabArchives notebook closely. If your absorption spectra have a weird flatlining at an absorbance around 3.0, you need to dilute your sample more.
(Week 2.) This week's experiment is relatively straightforward---you'll be making calibration curves for one of your nanoprism solutions from last week, as well as making silver-coated vials. Remember to clean your vial with ethanol beforehand, or the silver will not coat the inner surface of the vial properly.

Thought question: Can you explain the different colors of your nanoparticle solutions using MO theory?

Lab 4


Lab techniques: None.

Lab notes: You are welcome to start work on this lab at home, but you must still attend lab.
Here are some more details about what I'm looking for in terms of your lab report. Please also look at Lab 2 feedback below for more guidance. You should go to my office hours if you have specific questions or want me to provide (limited) feedback on your lab report before it's due. Bring a paper copy of your report. Turn your lab reports in on time! Late lab reports are worth half credit if turned in up to a day late and no credit if turned in later. This is not an easy assignment. But it is part and parcel of scientific work, and I encourage you to treat this as though you were communicating your results to a fellow scientist, instead of just an annoying assignment you have to complete.

Thought question: How would you construct the molecular orbital diagram for \(\mathrm{BeH_2}\)? For \(\mathrm{BH_3}\)?

Lab 3


Lab techniques: Vacuum filtration, syringe filtration.

Lab notes: There is significant downtime during this lab while waiting for your plant sample to be digested. During this time, we will discuss how to write a good lab report, and everyone should leave with at least a good hypothesis written describing a prediction regarding the trace metal content of the poisoned sunflower relative to the normal sunflower and explaining the rationale behind such a prediction. I also suggest, but will not require, that everyone work on writing their procedure for their lab report. Note that the discussion questions should be answered as a narrative in the discussion section of the lab report, not as an isolated list of questions and answers.
Thought question: The spectra obtained from an ICP-AES instrument are very clean, and the emission lines quite discrete. What distinguishes the ICP-AES spectra from, say, UV-Vis absorbance spectra, which are instead continuous?

Feedback from last lab:
Pre-lab:
A lot of you lost easy points because you did not show explicit dilution calculations for all your copper nitrate solutions, as was required. Please read and follow the directions for the pre-lab more carefully.
Lab notebook:
Overall, I'm pretty happy with the state of all your lab notebooks, and am confident that all of you now know how to take good observations. As a result, starting from this week's lab, you no longer have to show me your lab notebook before you leave lab. I will, however, still be grading you on your observations.
Common mistakes in the lab notebook included
Post-lab:
Note that the energy levels can only be characterized by just one quantum number, n, when all orbitals have the same energy, as is the case with hydrogenic (one-electron) atoms. In this case, however, Li, Na, and K are all multi-electronic species, and the orbitals have different energies. It's therefore not appropriate to say that the ground state is n=2---instead, it's the 2s orbital---or that the excited state is n=2---instead, it's the 2p orbital. And so on.

Lab 2


Lab techniques: Bunsen burner, flame test, spectroscope, dilutions.

Lab notes:
Thought question: What is fire?

Feedback from last lab:
Lab notebook:
I was not very clear regarding my expectations for the lab notebook, and I apologize. I graded last week's work more leniently to account for this. I will only grade things written in your lab notebook while you are in lab. When I grade your lab notebooks, I look at the last version of your notebook saved during the lab period. If you edit your lab notebook after lab, that's fine, but it will not affect your grade. All observations, measurements, and data must be taken and recorded during lab.
For observations, I expect at least six to eight sentences or bullet-point equivalents. Many of you asked what observations to write down. You should record
Common mistakes in the lab notebook included
Procedure:
Your procedure is for you. Write it in a way that will help you during lab. If the procedure tells you to weigh or measure something, have a blank line in that step of the procedure to remind you to record measurements. If there are important or time-sensitive steps, bold them. You can even write down all the glassware you need at the top of the procedure and get them all ready at the start of lab. Read through the post-lab questions beforehand, and think about what you need to pay attention to in lab.
A few of you decided to take multiple absorbance readings for each sample. This takes more time, but is a good idea in general. If you have extra time, all of you should consider doing this, especially for the upcoming written reports where having good data is more important.

Post-lab:
Individual feedback is included in the post-lab grading that you'll be able to view by Monday at the latest. Many of you did not include the equation for the best-fit line in the graph itself and did not show full calculations for every question. You should also pay attention to significant figures, although I did not mark you down for them this lab.
There were two different methods available to calculate the absorbance---to use the value of \(\epsilon\) obtained from the slope of the best-fit line, or to use the equation for the best-fit line directly. In principle, the best-fit line is preferable, because it represents your data best. Using the value of \(\epsilon\) corresponds to arbitrarily shifting the best-fit line up or down so the intercept is at the origin. In addition, whenever you are asked to compare two results (here, in Q7), you should be prepared to explain any discrepancy observed.

Lab 1


The first day of lab is Thursday, 10/4.
☞     Before your first day of lab, you must obtain lab goggles and a lab coat. See the relevant announcement on Canvas. You must wear close-toed shoes and long pants to lab, or I cannot let you in. Clothes made of synthetic fibers, like yoga pants or leggings, should not be worn to lab.
☞     You must also obtain a copy of Microsoft Excel or similar graphing software. Google Sheets is not accepted.
☞     In addition, you must complete the online safety quiz perfectly and academic integrity agreement by midnight of 10/3.
☞     You must complete all pre-lab questions before you can begin lab! The pre-lab is due an hour before lab starts.
☞     Tech is hard to navigate, so be prepared. You can try using this site. Don't be late for lab, because I have to give a lab lecture to everyone before we can start.

Lab schedule for week 2: Lab tour. Safety. Lab equipment and locker inspection. Lab. All labs will be performed in pairs, which have been randomly assigned. I will let you know who your lab partner is on the first day of lab.

Lab techniques: measurement, serial dilution, UV-Vis spectrophotometry, calibration curves, regression and data analysis.

Lab notes:
☞     Volumetric flasks have to be obtained from the stockroom. Every pair should pick up one 50 mL volumetric flask and one other (hopefully smaller) volumetric flask.
☞     Balances aren't very good, so the calibration curve won't be accurate due to the large uncertainty in concentration.
☞     Copper nitrate is deliquescent, which means that it absorbs moisture from the air and becomes sticky and hard to transfer. If the copper nitrate containers are left uncapped, the resulting copper nitrate will be hydrated and lead to inaccuracy in the concentration of your solution. Make sure you keep all copper nitrate containers capped at all times.
☞     Write about a full paragraph (6-8 sentences) for observations---for example, you can describe what solid copper nitrate looks like, what it looks like when you dissolve it, and what happens to the color when doing serial dilution, and so on. This lab isn't very exciting, so writing observations may be harder here. Note that observations are due by the end of lab, before you leave.
☞     If you run the spectrophotometry software on your computer and you get a sensor error, hold down the power button on the spectrometer until a blue light starts flashing, then let go. Close and reopen the spectrophotometry software. Some computers don't actually have this software, and in this case you should switch to a different computer.
☞     Calibrate dark means calibration without a cuvette in the spectrometer. Calibrate reference means calibration with a cuvette with DI water in the spectrometer. You should do both.

Thought question: Molecular excitations occur among discrete energy levels with well-defined energies. Why, then, is the absorbance spectrum continuous rather than discrete?