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Abstract SCHIRACK, ANDRIANA VAIS. The Effect of Microwave ...

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SAFE (3 SAFE's can be done in 1 day)<br />

(If the sample was in the freezer overnight, allow it to warm up early at RT)<br />

1. Make sure blue ball valve on vacuum system is closed (nearest to pump).<br />

2. Turn on the rough pump to achieve 10 -2 Torr (turn on gauge), and plug in the fan.<br />

3. Fill waterbath with 40-50°C water and plug in so it can warm up.<br />

4. Assemble the SAFE apparatus:<br />

Put Teflon threaded pieces and associated o-ring on any glass part without<br />

threads. Also, a sample stopper and stopcock are needed.<br />

<strong>The</strong>re are 4 parts to the SAFE: a round bottom flask, elbow, trap, and the<br />

main unit.<br />

Connect elbow and trap, and clamp into place.<br />

Attach this to the second trap (leave in dewar). Put traps as deep as possible<br />

into dewars.<br />

Make sure configuration is completely horizontal, and then loosely attach<br />

SAFE apparatus to ring stand. Fit nose <strong>of</strong> SAFE into neck <strong>of</strong> trap.<br />

5. Open blue valve slowly to 1/2 way, and wait to stabilize. <strong>The</strong>n connect SAFE – if<br />

it’s not going in easily, change angle <strong>of</strong> the SAFE apparatus. Use the vacuum to<br />

pull the SAFE into place. Avoid applying torque while attaching SAFE to trap -<br />

screw in and back <strong>of</strong>f as necessary. Tighten as much as you can by hand (use<br />

gloves).<br />

6. Wait until pressures stabilize to 10 -2 Torr, then turn on the small diffusion pump<br />

(small metal switch).<br />

187

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