An apparatus for handling reactive liquids - Journal of Chemical

An apparatus for handling reactive liquids. M. C. Waldman. J. Chem. Educ. , 1969, 46 (6), p 364. DOI: 10.1021/ed046p364. Publication Date: June 1969...
0 downloads 0 Views 460KB Size
University of British Columbia Vancouver 8, British Columbia Canada

I

An Apparatus for Handling Reattire liquids

I

W e have found the apparatus shown in Figure 1 to be very useful in handling air-sensitive and highly reactive liquids during their purification by vapor phase chromatography (vpc). The sample to he purified can be condensed under vacuum into the large finger. The pressure over the sample can he equalized by filling the vacuum with nit.rogen. This can be done either by using a nitrogenfilled dry box or by attaching the tapered-joint to a nitrogen cylinder. Tipping the apparatus at right angles lets the liquid run into the sampling finger; standing the apparatus upright allows the excess liquid to drain hack into the larger finger, and leaves the sampling finger full (-1 ml). A sample can he removed immediately for purification by using a vpc syringe. Any suitable lubricant can be used for the stopcock. Stainless steel Swaglok fittings (Fig. 2) have been found to be most inert. The Swaglolc fitting ('/An. bore) must he hollowed out slightly to accommodat,e the glass insert which we have in metric sizes only. The Swaglok is attached to the glass with Teflon ferrules. 'I hese ferrules (L/4-in.i d . ) are slightly smaller than the glass 0.d.; however, if they are heated slightly

in an oven they will then fit easily and form an air-tight seal. Vpc silicone septums are air-tight, permit multiple injections, and are essentially inert. The apparatus should also be convenient for use with gas samples. I n this case, the stopcock must be replaced with a Teflon screw-down valve (FischerPorter type) and a gas sampling syringe must he used.

cations for construction of system for hondling reactive liquids during "LL 8"

Nationd Research Council of Canada Studentship Recipient, 1967-68.

364

/

Journal of Chemical Education

LULL

UEA8YrlE*S*T$ ccMT,ME,Ees,

=,"EN

pY,iACatiOn,

for the opparot~s.