Kate's Inorganic Lab Blog

The purpose of this blog is to detail my experience in CHM4610, Inorganic Lab. Now that the semester is almost over, I feel I have made significant progress with understanding the basics of inorganic chemistry.

[katesinorganiclabblogthing]

Module 1 Assignments

I have been given brief instructions on how to write each section of a lab report in the past, but I haven’t had the opportunity to submit each section individually to see how I could best improve my writing. The introduction section is always the most difficult for me to write.

After this semester, I have learned that it is less difficult when I complete the discussion of my data first. I found that I needed a significant amount of background information to properly analyze my results, and practicing the concepts before writing my introduction increased my understanding.

[katesinorganiclabblogthing]

Information Literacy

I enjoyed researching an inorganic topic of my own choosing, which was lanthanide-doped nanoparticles that have applications for cancer therapy. I previously wrote a report on PFAS degradation via piezocatalysts, so I liked the opportunity to study a new topic from a different field within inorganic chemistry. 

I also learned about constructing an annotated bibliography and presenting my findings in an infographic to give a visually pleasing summary of the articles I read.

[katesinorganiclabblogthing]

Experiment 38

Organoplatinum complexes made up the last experiment of the semester. This experiment was beneficial to me because I was able to practice both H-NMR and C-NMR after not using either for a while. I liked that I was able to practice NMR because it could be a useful skill to use throughout my career, and it is important that I at least know the basics of how it functions.

I struggled with the synergistic bonding exhibited by the platinum and alkene, but I tried to make it the focus of my report. My report's introduction discussed synergistic bonding (aka backbonding) as well as a brief background on how NMR functions. To support any conclusions drawn from the NMR spectrum, an IR spectrum was also taken.

[katesinorganiclabblogthing]

Experiment 37

Experiment 37 was another synthesis of cis and trans isomers. This week's isomers included cis and trans-dichloro(dipyridine)platinum(II). The image above depicts the symmetries of the isomers and how they vary.

I determined the cis-isomer belonged to the point group C2v, and the trans isomer belonged to D2h. I attempted to highlight the axes and planes of symmetry with ChemDraw so that I could use them to explain my reasoning within my introduction.

I used IR spectroscopy to determine whether the isomers were successfully produced and compared their symmetries to differentiate between the spectra.

[katesinorganiclabblogthing]

MOFs

This experiment synthesizes ZIF-8 and ZIF-67 complexes, both types of metal-organic frameworks (MOFs). Several different types of analyses were run this week to determine whether the experiment was successful.

I studied the particle sizes with SEM, solid-state UV-Vis, magnetic susceptibility, IR, X-ray diffraction, and TGA of the complexes. I have not used X-ray diffraction, solid-state UV-Vis, or SEM before, so I gained a lot from this experience.

I appreciated that I was not only able to practice analyzing the data for these new techniques, but I was also able to run the XRD and observe the solid-state UV-Vis.

[katesinorganiclabblogthing]

Experiment 49

Today I synthesized cis and trans-bis(glycinato)copper(II) monohydrate. This topic allowed me to review the basic topic of thermodynamic and kinetic products, which were first discussed in organic chemistry. 

I tried to focus my lab report on the differences in symmetries (shown in the image above), which determine the point groups and vibrational motions of the complexes. I found it difficult to explain these differences with the IR spectra, but I ended up using the location of the carbonyl peak around 1720 to describe symmetry’s effect on the complexes. 

[katesinorganiclabblogthing]

Silver Nanoparticles

The silver nanoparticle experiment is probably my second favorite. I enjoyed watching the solution's color change as the reaction progressed.

I was able to obtain the blue color expected for the KBr concentration, but the UV-Vis and reaction rate data did not appear correct. It's possible that the reaction was contaminated or the UV-Vis was performed incorrectly. The poor reaction rate was probably because I over-diluted my solution.

Writing this lab report helped me learn about plasmonic resonance and how color can be selected based on reactant ratios.

[katesinorganiclabblogthing]

Quantum Dots

Of all the experiments this semester, this was my favorite. It was also the first full lab report, so I tried to improve my transitions when putting my background, data, and analysis together.

I synthesized CsPbCl3, CsPbBr3, and CsPbI3. CsPbBr3 is shown above, but CsPbCl3 and CsPbI3 did not appear as expected. The UV-Vis for all products were different than expected, so this experiment was likely unsuccessful or contained significant impurities.

[katesinorganiclabblogthing]

Experiment 47

Experiment 47 focused on saccharin complexes with cobalt and copper. Product A was tetraaqua-bis(o-sulfobenzoimido)copper (II), and product B was tetraaqua-bis(o-sulfobenzoimido)cobalt(II).

To analyze the product, I used IR, UV-Vis, and TGA. This was my first time using UV-Vis for this lab, although I have experience outside of class. It was interesting to see how different types of spectrophotometers function. I have used a different form of UV-Vis for my organic lab, and another at my internship, so I enjoyed learning about the different software.

After lab, I learned about the process behind writing introductions for lab reports. I typically write my introduction section first, but I have never been taught what exactly I should be discussing. I'm glad I was able to get feedback on what is actually important to an introduction.

[katesinorganiclabblogthing]

Experiment 22

"Today," I synthesized metal acetylacetonates. The expected products were tris(2,4-pentanedionato)chromium(III) and tris(2,4-pentanedionato)manganese(III).

For this experiment, I got to practice calculating the magnetic moment given the magnetic susceptibility. I believe my calculations improved a lot after studying a walk-through of an example magnetic moment calculation.

My yields were overall slightly better than the previous experiment. I had a yield of 23.08% for product A, and 56.61% for product B. I was able to get melting points close to their expected ranges, so the little product synthesized was likely pure.

I was also able to build on my knowledge of IR peak identification for this experiment.

[katesinorganiclabblogthing]

Experiment 20

For the second experiment of the semester, I synthesized metal complexes of dimethyl sulfoxide. There were 3 products: CuCl2*2DMSO, PdCl2*2DMSO, and RuCl2*4DMSO.

Parts A and B only involved stirring the solution before vacuum filtering. Product C involved refluxing the solution before reducing with a stream of gas. After reducing the solution, acetone was added, and the mixture was cooled. Finally, the solution was filtered, and all of it went straight through the filter.

For product A, 55.60% of the expected product was obtained. Product B yielded much less, 7.98% of the expected yield. Product C was not successful; no crystals were collected with vacuum filtration.

While part C was not successful, I learned more about determining the melting point for products A and B. Enough product was made, so I was also able to analyze the IR spectroscopy.

[katesinorganiclabblogthing]

Experiment 17

MIMT is portrayed in the above photo, and it can form an octahedral complex Co(mimt)4(NO3)2*H2O and a tetrahedral complex Co(mimt)2(NO3)2 with select reactants.

In order to differentiate between the two complexes, IR spectroscopy, melting point, and magnetic susceptibility were recorded.

Melting point and magnetic moment determination are two methods of analyzing a substance's purity that I had yet to complete. Calculating the magnetic moment based on the magnetic susceptibility was the most difficult, in my opinion, but I was familiar with IR spectroscopy.