Add 2.0 g of 30 mesh zinc granules and a stir-bar to a Schlenk tube. Connect the Schlenk tube to the Schlenk line and flush with nitrogen. Add 18 mL of 0.1 M HCl to the zinc, cap the tube with a septum, and let it stir for about 5 minutes. Meanwhile, prepare a solution containing 9.0 g CrCl₃.6H₂O in 16 mL of 0.2 M H₂SO₄. Remove the septum under nitrogen pressure, and add the CrCl₃ solution. Replace the septum and continue stirring. In the meantime, combine 12.35 g sodium acetate trihydrate and 25 mL of water in a second Schlenk tube. Add a stir- bar and de-gas the solution by flushing the tube and solution with nitrogen. Then cap the tube with a septum. By this time the zinc should have completely reduced the Cr(III) to Cr(II) and the solution should be a bright blue with no traces of green. Transfer the Cr(II) solution to the stirring sodium acetate solution using the cannula, as shown in Picture 1. A brick red precipitate should form immediately. Write the equations for the reactions that have taken place in your notebook.

Under a stream of N₂, assemble the apparatus as shown in Picture 2. Carefully flip over the apparatus (try to get as much product into the Schlenk frit as possible). Remove the liquid by applying a vacuum to the lower Schlenk tube and opening the lower stopcock. De-gas 10 mL of ethanol using a fritted glass tube to bubble N₂ through the liquid for 4 minutes. Remove the upper Schlenk tube from the apparatus and add the methanol to the product. Swirl momentarily, and then let drain. This removes most of the water. Wash the product with 10 mL of degassed diethyl ether (de-gas in a similar fashion as the methanol). Cap the Schlenk frit with a Schlenk cap and apply vacuum to the Schlenk frit. Wrap electrical tape around the cap and joints of the Schlenk frit to prevent them from blowing off in the dry box. Pre-weigh a large ampule. Put the ampule, a stopcock and rubber tube (make sure the stopcock is open), the Schlenk frit, a spatula, a 100 mL beaker, and a rubber funnel into the antechamber of the glove box. Pull a vacuum for 5 minutes. Backfill with N₂ from the box, and pull a vacuum. Repeat this operation two more times. Open up the inside door to antechamber using the gloves and transfer all the materials placed in the antechamber into the glove box. Close the inside door to the antechamber. Now you are ready to transfer the solid into the ampule. Open the Schlenk frit and transfer the solid to the beaker (do not scrape the Schlenk frit too hard). Transfer all of the product except for a small amount to be used for mass spectrometry to the large ampule using the rubber funnel to assist. Slip the stopcock/rubber tube on the ampule, and close the stopcock, as shown in Picture 3. Now, open the inside door to the antechamber, place all materials that you brought into the glove box into the antechamber, and close the inside door. Now, open the outside door and remove your materials, including the ampule connected to the closed stopcock. Connect the stopcock to the Schlenk line and apply a vacuum. Open the stopcock SLOWLY. Seal the ampule using a gas/oxygen torch. Weigh the ampule and the remaning glass pieces. [NEED TO ADD THE PROCEDURE FOR PREP of MS SAMPLE!]