The overall goal of this procedure is to prepare functionalized delta rals into clusters of germanium di vinyl. First to prepare the precursor load pure metallic potassium and germanium into a opium tube and seal by arc welding under a vacuum. Enclosed the niobium reaction vessel in a FU silica tube and heat in a 950 degrees Celsius furnace.
After dissolving the inter metallic compound in ethylene diamine alate to functionalize delta head intel clusters, ultimately electros spray mass spectrometry and crystallization results confirm the successful formation of functionalized germanium di vinyl clusters. This method can provide insight into the alkalinization of nine atom delta germanium zeal ions. It is also applicable to various systems such as various nine ATI Intermetallics function lines with various organic subsid such as alky, halides, and al kinds.
Measure four segments of the niobium tube of 4.5 centimeters in length, cut with a pipe cutter and place into a beaker, poor niobium cleaning solution to completely cover the tubes. Close the sash of the fume hood until brown nitrous oxide gas is released. Then immediately fill the beaker with water with plastic tongs.
Remove the niobium tubes, wash several times with water and acetone. Then dry in a high temperature oven. When called, use vice grips to crimp about one centimeter of one end of each tube and slightly bend the edge about one millimeter.
Then c clamp the four niobium tubes in a staggered position in an arc welder's holder, adjust the welding tip to the height of the niobium tubes. Place under a partial vacuum position, a protective welding darkened glass as the welding tip makes contact with the niobium tube to form a welding arc. Raise one centimeter over the tube and slowly sweep above the tube to seal completely.
Continue to seal all tubes with an electrical engraver. Label the opium tubes dry in an oven. Then evacuate the hot tubes in the anti chamber of a dry box with a spatula.
Carefully insert four millimoles of potassium into each opium tube and push to the bottom. Then overlay with nine millimoles of germanium. Carefully crimp the open end of each opium tube using vice grips and slightly bend the edge.
Place all four tubes in a jar under inert gas and place it in the box anti chamber. Proceed to weld the edges of the loaded tubes with a circular glass saw. Cut 10 to 14 inch pieces of large and medium quartz tubes.
Also cut an end of a round ball joint wash pieces thoroughly with water and acetone completely dry them in an oven. Next lighter, a hot blue flame to a hydrogen oxygen torch. Insert a large silica tube into the flame and slowly rotate one end for the tube to collapse into a bottleneck.
Using a medium quartz tube, shape the white hot end and seal the opening. Now attach a rubber septum connected to a blow hose and position the blow pipe into the mouth while rotating the sealed end in the flame Blow lightly to keep positive pressure and prevent the glass from collapsing. Then adjust the gas flow to create a sharp blue flame.
Focus the flame to the center of the closed end. When the targeted spot becomes white hot, blow hard to create a large bubble or opening. Break the bubble by gently scraping on a lab bench.
Next, insert the open hole into the flame and flare the edges with a graphite reamer to open to one centimeter. Also close one end of the neck piece with a rubber septum proceed in the flame to slowly rotate neck and body pieces simultaneously to attachment straighten outside of the flame. Now with a septum, close the ball joint opening and attach it to the neckpiece.
Then insert the four loaded niobium tubes. Attach the end of the blow hose to the ball joint and slowly seal the body. After cleaning.
Seal below the ball and neck joint under a high vacuum line to case the niobium tubes in a fus silica quartz jacket. After heating the reaction tubes in a 950 degree Celsius furnace for 48 hours, remove the tubes when called to room temperature with wire cutting pliers. Cut the ends of the niobium tubes to release the fine inter metallic precursor.
Weigh out 81 milligrams into a test tube and stir in two milliliters of anhydrous ethylene diamine to dissolve into a bright red solution containing delta germanium clusters. In a dropwise fashion, add ALK agent to form a clear honey brown solution. After centrifugation, harvest the filtrate of organal iron, evaluate a sample by electro spray mass spectrometry analysis in negative iron mode, and obtain an isotope pattern.
For the functionalized clusters, add eight milliliters of toluene to 105 milligrams of anhydrous 18. Crown six, mix well until completely dissolved. Now divide the filtrate preparation into two clean test tubes.
Carefully layer each with four milliliters of the toluene solution of 18. Crown six. Place a rubber stopper and set aside undisturbed to crystallize into bright orange blocks.
For single crystal x-ray diffraction. Transfer select orange crystals into perone N oil. Under a high resolution microscope, select a single crystal and drag it to the edge of the oil on the slide with a straight stainless probe.
Proceed to evaluate the crystal under the cold stream of a refractometer equipped with a CCD area detector. Ensure good high angle diffraction and acquire unit cell ESMS spectra of delta ral. Germanium clusters indicate a unique isotope pattern easily detected in the negative iron mode.
Furthermore, the orange crystalline blocks can be further detailed by single crystal x-ray diffraction. After watching this video, you should have a good understanding of how to synthesize by high temperature, very air and moisture sensitive inter metallic compounds containing highly reactive elements. How to extract zeal anion in solution from the inter metallics and how to functionalize designs.
The techniques shown in the video include arc welding, quartz, glass blowing, and handling of air sensitive compounds.
