Surf Diaries 2006

Only a few more weeks of SURF and I still have so much work to do.  Unlike a lot of other SURF projects, in both science and art, my project does not have a set 'stopping point.'  My project is to synthesize different compounds, of which there are countless possibilities.  Because of this, I can't simply finish my project in a week and spend the rest of the time writing a paper.  I'll be doing experiments up until the day my poster is due, and working on my paper outside of lab time.  Lizzy has this problem too.

Last Thursday and Friday my stuff worked, for the most part, and I was able to synthesize the compound I want.  Unfortunately, I can't get the compound out of solution.  For the beginning of this week I'll be trying to crash it out with different solvents, and trying different procedures, to see if I can get it in solid form.

The new glove box is almost up and running, which is great.  I'm waiting for PtCl₂(dcpm) to mix for another 10 min, while lizzy and Dr. Schreiner are figuring out how to use it.  It's an upgraded version, so it has a lot of new features we're not used to.

As a side note, the NMR that we all fight over is broken again.  This isn't unusual, it has minor problems all the time that either Dr. Schreiner or Dr. Thobourn can fix.  Today's problem is much harder though. They think the acquisition computer is broken and they don't know why.  So, if anyone reading this has $0.5 million dollars they want to give us so that we can buy a new NMR, that would be great.  Send any donations to Dr. Schreiner.  Thanks!

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Today's lesson will be about preparing solutions to go into the glove box.  I think I posted this earlier, but here's a review: a glove box has an inert environment of nitrogen gas.  Chemicals that are pyrophoric (combustible when exposed to oxygen) are stabilized in the glove box by bonding to other chemicals.  Because the glove box cannot have any oxygen in it, we have to prepare solutions and solids before they can go into it.  Solids are weighed out and placed in vials, with the lids almost tight.  Liquids are sparged, then freeze-thawed 3 times.  In analytical chemistry, 3 is the magic number: glassware is washed 3 times, weigh-boats are rinsed 3 times, and liquids are freeze-thawed 3 times.  There are three ways to purify a solvent: sparging, freeze-thaw, and distilling or running it through a column.  Sparging is the term for bubbling another gas through the liquid, in order to displace the undesired substance.  When you freeze-thaw a liquid, you freeze it, then vacuum out any air in the flask.  You then thaw it, and repeat the process.  It's not a hard process, but takes a fair amount of time when you have more then two flasks.  When everything is ready to go into the glove box, you put it in a vacuum chamber attached to the box.  You vacuum out the air for ~30 min.  After all of this is done, you are finally ready to do your experiment.

The great thing about our new glove box is the built in solvent dispenser.  Once it is all set up, there will be 5 solvents connected directly to the box, and we won't have to freeze thaw any more. 

This morning I filtered three reactions, and then helped lizzy get 6 flasks ready for the glove box.  Although this doesn't sound like a lot of work, it's taken all morning.  This afternoon I think I'll be reading more journals.  Either that, or going over procedures to see if I can increase the percent yields.

Well, I'm off to lunch.  Hope you're all having a great day!

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This weekend Lizzy and I painted all of the cabinets in lab.  Michelle came in on Saturday to help with the primer, but her wrist started to hurt too much.  Lizzy and I came in on Sunday to paint the first coat of paint, and then came in later that night (after the world cup final) to paint the second one.  Michelle had a really good idea to use chalkboard paint on the cabinets so we could use chalk to label the contents, rather then making labels and have to scrape them off every time we rearranged them (like we were currently doing).  Lizzy and I peeled off the old labels, and found Dr. Marchetti's handwriting underneath.  For those of you who don't know, Dr. Marchetti went to RMC as an undergrad and now teaches here (after getting her doctorate from Penn State).  The paint had to dry for 3 days before we could write on them, so we're going to test it out later today.

Experiments are going okay.  I seem to have good days, where everything works, quickly followed by bad days, where nothing works.  Dr. Schreiner found a different procedure to make Pd COD, it's much faster then the old way so I'm a fan.  I'm currently trying to synthesize Pt₂(dcpm)₃ and Pd₂(dcpm)₃.  I have a few different procedures, but none of them seems to work.  The way we're going about making the compounds is to research and find procedure for similar compounds, and see if I can make my compounds the same way.  Once the compound is successfully synthesized, we then try to see which the easiest and cheapest procedure is, or which one produces the highest percent yield.

Another project Dr. Schreiner and I are trying to figure out surrounds the two compounds PdCl₂(dcpm) and [Pd(dcpm)₂]Cl₂.  According to the literature, the double-chelated compound shows and NMR peak at -34.3.  I have synthesized this compound successfully, but I cannot seem to synthesize the mono-chelated one.  Using the same procedure for Pt mono-chelated compound, I still get the -34.3 shift.  Hopefully I'll be able to find out what's going on.

Monday we had another game of soccer, only this time it was against some guys from the RMC soccer team.  We decided to make it a weekly game at 5:30, so if any of you are in the area, feel free to come on over.

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Coming back to work after the 4 day break was pretty hard.  Wednesday was a pretty slow day for all of us.  I ran NMRs and IRs all day, in addition to searching for articles on SciFinder, instead of doing any experiments.  SciFinder is a program that allows you to search many scientific journals for chemical structures, chemical formulas, research topics, author names, publication date, and more.  One important aspect of research is to continually research what's going on in the field.  The last thing you would want to do is spend months or years researching a topic and then find out that someone has already published the same thing.  Another reason they can be helpful is that they can give you ideas for different reagents, solvents, or syntheses.

Yesterday was a pretty successful day of synthesizing.  One more experiment, and I'll finish up my work with this series of hydrides.  Dr. Schreiner found some interesting experiments to try in addition to what I already have planned, so I will begin work on that Monday.  Friday seems to be the day when I end up making more starting material.  Last night I stayed late synthesizing more K₂PtCl₄, and today I'm making more Pd(dcpm)Cl₂ and PdCl₂COD ( I made Pt COD last Friday).  I've only made Pd COD once, and used a different procedure.  Today's experiment started off well, with a brown soln. turning yellow as it was gently heated.  However, gray solid looked to be precipitating out of soln.  This is bad because it usually means that the metal has been reduced, and can no longer be used.  However, there is still yellow solid in the soln, so there's still hope.  I'm letting the rxn cool to room temp and will then filter it, and go from there.

On an unrelated note, Michelle's wrist turned out to be broken.  Unfortunately, she can't continue her project (she broke her right wrist and is right-handed).  She's now working for admissions, so if you plan to come visit the school, stop by and say hi.

Last weekend at the lake was fun.  We all got pretty tan, which was nice.  This afternoon a lot of the SURF people are going to play a game of pick up soccer, organized by the P-Chem professor (Dr. Michelsen).  After that, the SURF program is paying for us to go see the new Pirates of the Caribbean movie at Short Pump.  Tomorrow, Sat., Lizzy and I are coming in to lab to paint the cabinets.  They are an awful yellow-mustard color from the 70s.  I have no idea how anyone thought it was a good color.  We're planning to paint them with chalkboard paint, and then use chalk to label the contents.  We'll see how that goes'   Hope you all had a great 4^th of July, and I'll update sometime next week.

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This week has been great for my research lab.  My lab group started coming in at 7:30am instead of 9.  With this extra morning time, we have all been able to get a lot more work accomplished.  We no longer have to wait for mid-day to check compounds, we have been able to check them in the morning and then work with them the rest of the day.  I was able to successfully isolate my hydride compound from last week and will begin doing reactivity studies next week.  I'll react it with a series of sulfur-containing compounds to test its ability to insert sulfur between the metal-metal bonds.

Last Friday our new glove box was delivered.  A glove box has an inert environment of N₂.  It doesn't have any air in it, so we use it to stabilize pyrophoric compounds.  Up until now I haven't needed to use it, but one aspect of my research is comparing the reactivity of different phosphorus ligands, so I will need to use it soon.  I have used dppm (bis(diphenylphosphino)methane) and dcpm and (bis(dicyclohexylphosphino)methane, both of which are relatively air-stable, and do not require a glove box.  However, next week I will start work using dmpm (bis(dimethylphosphino)methane) which is pyrophoric.

I'm currently waiting for a compound to dry in the oven, and then I'm done for the day.  Michelle hurt her wrist, so she can't work today, and all of Lizzy's stuff are 2-day experiments, she can't start anything today either.  Therefore, they are both starting the holiday weekend early.  Dr. Schreiner also left early for Boston.  I'm going to Lake Gaston, about an hour and a half away tonight, and will stay until Tuesday afternoon.  Hope you all have a great weekend!

P.S. I told Sami and Emma I'd mention them in the entry, since besides my mom I think they are the only 2 people reading it.

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Today ends the second week of SURF, and more importantly, pay day.  I am currently waiting for a compound (K₂PtCl₄) to dissolve in deionized water.  Once it is all dissolved I will filter the soln., add acetic acid and COD and eventually precipitate out PtCl₂COD.  PtCl₂COD is one of the main starting materials for all of mine and Michelle's compounds.  Work has been going okay.  I was having a problem with one of my compounds, but I finally figured out the problem.  Well I should say Dr. Schreiner figured out what was wrong.  NMR time has still been hard to fight for, but Lizzy, Michelle, and I are going to come in at 7:30 starting Monday.  Everyone else doesn't come in until 9, so we'll have some extra time then, and we can also get on when everyone else takes their lunch break.

I really like doing research but it took me a few days to get back into it.  There are no windows in lab, so you are isolated from everything.  At times I miss being outside and getting a tan, but for the most part it makes it easier to focus.  One reason I really like chemistry is because it is so challenging.  Even if an experiment works 10 times, the 11^th time can give you trouble, and then it's like a puzzle trying to figure out what when wrong and how to fix it.

One of my current projects involves a hydride complex.  The solid should be colorless, but mine is brown.  According to NMR and IR (infrared) spectroscopy, I have the correct compound and it just has some 'junk' on it.  Because of this, I'm trying to get the white solid and the brown solid into 2 different states in order to separate them.  Unfortunately, they have similar chemistry, so separating them is proving difficult.  I do like that it makes you think.  I have a small amount of the solid, so I have to think about whether to use polar or non-polar solvents.  Well I have to go make sure my rxn. doesn't overheat.  Have a great weekend!

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Today I'm starting my second week of SURF.  Last week was busy, but not terribly productive.  My advisor was out of the country on Monday and Tuesday.  He and another professor were in Australia setting up a J-term class for the 2006-2007 school year.  My lab partners, Lizzy and Michelle, and I went into lab at 9am on Monday and unpacked some new lab equipment.  We then went to the SURF luncheon to hear about everyone else's projects.  We had Tuesday off and I used the time to unpack my apartment.  During SURF the students are allowed to live in the senior apartments (4 students per apartment). 

Wednesday we began to do experiments, however it wasn't so easy.  One of the machine's we use to characterize compounds is called an NMR (nuclear magnetic resonance).  It is always in demand, and with 8 chemistry students fighting over it, it's hard to get time on it.  Because of this, I was only able to do one experiment.  The rest of the day Lizzy, Michelle, Dr. Schreiner, and I reorganized our lab.  Thursday and Friday were similar to Wednesday, in that I could only run experiment per day.  This isn't the best news for my project, but on the bright side, the lab looks great.

Today we started lab at 9am again.  I wrote up some experiments, and began another.  Unfortunately, it is not going as planned.  Over the past year and a half of doing research, I have learned that it is very rare for everything in lab to go as expected.  I am currently waiting for a compound to dry, and then will analyze it through NMR spectroscopy.

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Right now i'm home in New Jersy enjoying the few weeks off before SURF starts. This weekend i'll be back at school to attend graduation, but i'll have another 2 weeks off before I get started on my summer project. Over the summer i am attempting to synthesize multinuclear platinum and palladium complexes, a continuation of my SURF project from last summer.

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