Degassing Samples of Low Volatility Deaersting liquid samples contained in narrow tubes, such a7 4-mm i.d., nmr, epr, and some photochemical and radiation-chemical sample tubes, can be an extremely t,edious and time-consuming task if freesepomp-thaw cycling of the liquid ha? to be carried ont in the t,nbe. Complete removal of the dissolved air is hindered by the unfavorably small swface area/volume ratio. Ideally, the liquid sample shoold he degaqsed elxcwhere in the vacuum system whero it can be manipulated and eventually returned to the tube by dixtillation [IIONDEAU, I ~ O G EE., R J. CHEMEDUC.,44,530 (1967)l. This isn't always possible, however. If the liquid has too low a. vapor pressure to permit liquid nitrogen VXUM SYSTEM pumping then another means of transfer within the vacuum system rnwt be used to ret,urn the dega-sed liqnid to thesample tube. Described below is s. quick and ossy method of NMR TUBE degassing liqnid samples wit,ll low volatility. A few ground g l a ~ sball and socket joints and s. minimal glass blowing ability are all that, is needed. The silmple tube is butt-sealed to the modified ground glms joint, A. After adding t,hc provionsly measured sample to the cup, B, the joint is then attached to t,he vacunm maniiold t,hroogh the adaptor, C. The sample is frozen by immersing the cup in a suitable coolant, such as liquid nikagen, and the entire system is evacuated. Now the liqoid can be efficienlly degassed by freoae-pump-thaw cycling since it exposes a.muoh greater surface area. After degassing, A is rotated 180' while C is held in place. With the tube pointing down, the sample is tramferred to the tube by gravity. There the liqrdd is fronen one more time for flame sealing. During the sealing-off operation, the valve to the vacuum system should remain open and tho pressure be continuously monitored. Any leak which should develop a t the seal-ofl point will then be readily noticed.
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AIR FORCE MATERIALS LABORATORY WRIGHT-PATTERSON AFB, OHIO45433
504
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Journal o f Chemical Educofion
