Chapel Hill, NC – As you know, Ben Kumpf (’18) and I are working in the Isotope Geochemistry lab at UNC Chapel Hill. We are measuring isotopes of strontium (Sr), lead (Pb) and neodymium (Nd) in basaltic pillow lavas from northern British Columbia. In order to measure the elements, we need to isolate them from the rest of the elements that make up our rocks. We purify individual elements using the method of column chemistry. A column is like a filter for elements; we pass our sample through the column and the column captures the element of interest, then we release and collect the element off the column to be analyzed later.
The first step to preparing our samples is to dissolve our rock powders in an acid solution. Ben Kumpf (’18) weighs small amounts of rock powder into Teflon vials. We add a series of acids to the vials and let them sit on a hotplate for a day or two until the powders are completely dissolved.
Once the samples are dissolved, we measure out a small amount of the solution into a new vial to run it through the column chemistry process. The first step to make a column “load” solution is to dry the sample solution down to a powder on a hotplate.
To the dried-down powder, we add an acid that is appropriate for the column that we’re using. For Sr, we’re adding nitric acid to the vials.
Now we’re ready to set up the columns. Dr. Ryan Mills (psychedelic lab coat) is showing Ben Kumpf (’18) how to add the resin.
This is what a column looks like up close. It’s suspended above a waste beaker. The white material that is filling the tube and neck is the resin. You can see it still settling out of solution. The resin that we use to isolate Sr was developed in response to the Chernobyl accident when it became necessary to remove radioactive Sr from milk (Vajda and Kim, 2010).
The chemical column process involves adding a series of solutions to the columns in a sequence that cleans the resin, conditions the resin for the sample load solution, introduces the sample, and rinses the sample through the resin. There’s a lot of pipetting and waiting for the solutions to move through the column during this stage.
Samples are centrifuged prior to loading. The centrifuge separates any undissolved solids from the liquid so that we only add the liquid portion to the column.
These columns are loaded with our Pb solutions.
Now that our sample has passed through the column, we release all of the Sr or Pb off of the column and collect it in our sample vial.
The last step in the process is to dry down the sample one final time. This makes a tiny bead at the bottom our vial. We will load this bead into a mass spectrometer to measure the isotope composition.
Now you can see why we need do our sample preparation in a clean lab.
Vajda, N. and Kim, C.-K. 2010. Determination of radiostrontium isotopes: A review of analytical methodology. Applied Radiation and Isotopes 68: 2306-2326.