Stephen Myers from the NSMS department graciously helped Alex and I out with the next phase of the FTIR experiment. He was able to get a hold of a couple of quartz cuvettes from Spectrocell. On top of that I had ordered one from Amazon.
The first part of the experiment required us to “blank” the samples so we put a Spectrocell cuvette into the FTIR machine and took a reading. For fun we then did the same thing with the Amazon cuvette and then compared the two curves.
While the two graphs look identical we noticed that the sample from Amazon had a weird periodic feature in the graph. Stephen said in other experiments he attributes this pattern to some kind of film, whether or not that is what is going on here is debatable. Regardless I decided to use the Spectrocells for the remaining experiments.
Before we began I thoroughly rinsed each cuvette with DI water and dried with nitrogen. This did not remove all the liquid water, but most of it. I attempted to air dry the remainder. This is important information for later. I used 3mL of each water type (DI, DDW, D2O, and a D2O/DDW mix) for analysis in the FTIR spectrometer. For the D2O sample and for the D2O/DDW mixture I used the second Spectrocell cuvette (which was not blanked) so that the high D2O content wouldn’t contaminate the DDW samples. I used the same cuvette for the DI, and two DDW samples (I’ll explain this in a second).
We took spec readings in this order: (first) DI water, D2O, DDW, D2O/DDW mix, (last) old DDW. I chose this really random order because we weren’t sure we would be able to get any interesting data so I wanted to see DI water vs D2O first. When that gave us obvious results we tried the first DDW sample (taken from a bottle that was opened 11/30/11). Then I wanted to compare all these results with a close to 50/50 mix of D2O and DDW (I didn’t pipette exactly 1.5mL of each nor can I report on how close to that number it is, I was merely trying to determine if there would be a difference between DI, D2O, and a mix of those two with a larger percentage of D2O). Finally we measured a sample of DDW that was taken from a bottle that was opened 9/6/11.
Here are those results.
Wowie zowie! The data display isn’t ideal (done in excel quickly) but you can see a difference between each of the samples. There is one exception that is actually remarkable. The sample of DDW from 9/6/11 matches really well with the sample of DI water. The newer sample of DDW (11/30/11) is more distinguishable from these two than it appears above. And the mixed sample and that of pure D2O are very distinguishable both from each other and from the other samples!
If you notice that just above 1.5um (wavelength) there are two tiny humps in the data. I have blown that up below.
Here there isn’t much different between the DDW samples and DI sample, but there is a difference between those and the DDW/D2O mixed sample. I didn’t include the D2O sample because the transmission in this range was much larger than these samples.
Now for the best part: Stephen was totally shocked that we were able to notice these differences. He wasn’t expecting much and frankly neither was I (I had been expecting to not notice anything because most papers I had read focused on the MIR range for FTIR). I was super stoked about these results, and happily, Alex was as excited about these results as I was/am!
I uploaded the graphs to Google Docs and all the data can be accessed here. I’ll upload the data to FigShare and link to that later.
Update: I forgot to mention that we are using a Nicolet 6700 FTIR spectrometer from Thermo.
Update (12/25/11): Fixed link to data. Thanks Koch