Monel vacuum line

Figure 2. Monel vacuum line for the preparation of radon compounds ...

Apparatus and Matoials. A Monel vacuum line was used. It was equipped with stainless-steel or Monel 1KS4 Kel-F tipped Whitey... 

A metal (stainless steel, nickel or Monel) vacuum line is constructed in a well-ventilated hood/ This line is equipped with a Bourdon tube gauge [Dresser Industries] with a range of at least 0-1500 torr. A small cylinder (0.5 lb) of fluorine [Matheson] is stored behind a suitable barricade [Matheson]. The cylinder is equipped with a standard two-stage regulator [Matheson] and then connected to the metal line via /4-in. copper, nickel, or Monel tubing. 

CAUTION. Fluorine is a strong oxidizer and a very corrosive material. An appropriate vacuum line made from copper or Monel in a well-ventilated area should be constructed for working with this element. The reactions themselves were carried out in Teflon vessels. If elementary precautions are taken, work with fluorine is relatively simple. 

Apparatus. The preparations may be carried out in quartz or Teflon vessels. A bottle of 30-ml. capacity and internal diameter 2.5 cm., provided with a standard-taper quartz joint, for attachment to a vacuum system is satisfactory. A small copper, nickel, Monel, or Kel-F funnel is needed to facilitate addition of liquid bromine trifluoride. Excess bromine trifluoride removed on the vacuum line must be collected in a quartz or Kel-F trap. Silicone or Kel-F vacuum grease must be employed in those parts of the vacuum system likely to come into contact with bromine trifluoride vapor. Vacuum grease should be applied to the cone of the quartz bottle only after... 

The apparatus used is shown diagrammatically in Fig. 14. The vacuum line is made from f-in. nickel or Monel tubing. The metal valves can be of the bel-... 

All of the compounds used or prepared in this work are spoiled by water. All transfer of materials was therefore carried out either in the dry atmosphere of a Vacuum Atmospheres Corp., DRILAB, or by distillation under vacuum in well-dried apparatus. All containers or exposed surfaces were of aluminum, Monel, Kel-F, Teflon or quartz. Vacuum lines were constructed of Autoclave Engineering 30VM6071 Monel valves (rated to 30,000 psl) and appropriate lines and connectors. Normal working pressures were measured with Monel Helicoid gauges — one for the 0-1500 torr range, and another for the 0-500 psi range. 

Vacuum System and Apparatus.—All preparations were carried out in Kel-F bottles or traps jointed to a 1/4 in. Monel tubing line by way of Swagelock compression fittings. The Monel line incorporated several Kel-F traps in series, for trap-to-trap distillation of the reagents and for the collection of volatiles from the preparations. 

Apparatus aad Reagents. A nickel vacuum line was used. It had a mercury diffusion pump, a mechanical pump, and soda-lime scrubbers (for removal of fluorine, HF, and oxidizing fluorides) and was equipped with a Monel Acco Helicoid pressure gauge (0-1400 Torr, 0.3%) and nickel valves with Teflon packing. Teflon FEP reaction vessels (18 mm o.d.) equipped with Teflon valves were used for all preparations. Agp2 (99.5% purity Fluka, Buchs, Switzerland) was used as supplied. KrFj... 

Apparatus.—Most preparations were carried out in a stainless steel cell attached via Swagelock fittings to a stainless steel Whitey IKS4 valve. Some reactions were carried out in FEP (Chemplast, Inc.) tubes. All of the solid materials were handled in the dry atmosphere of a Vacuum Atmospheres Corporation Drilab. Volatiles are manipulated with a Monel-metal and stainless-steel vacuum line provided with Autoclave Engineering 30VM-6071 valves. 

All hydrogen halide samples are purified before use HCl, HBr, HI (Matheson Gas Products), and DCl (Merck) are condensed at 77 K, pumped on, and then distilled to remove parent halogen impurities HF (Matheson), which is handled in a copper vacuum line fitted with Monel valves, is condensed at 196 K and pumped on to remove SiF. ... 

The procedures for the preparation of thionyl tetrafluoride and pentafluorosulfur hypofluorite are essentially the same, with one important difference the use of a catalyst. The apparatus employed in the preparations consists of several Monel pressure vessels (which have been prefluorinated at 150-200 ), a standard glass vacuum line equipped with several large calibrated storage bulbs (1- or 2-1.), a partial fractionation train, and several ball-joint connections on the main manifold. All the joints and stopcocks on the vacuum line are lubricated with Kel-F-90t grease, and all mercury manometers are covered with Kel-F-10 oil,t which has been well outgassed. The vacuum line is connected to a fluorine metering system and a water... 

A storage cylinder containing thionyl fluoride is attached to the manifold of the vacuum line by means of a ball joint, and the thionyl fluoride is allowed to expand into one of the calibrated storage bulbs. After 0.021 mole of thionyl fluoride is collected in the bulb, the excess in the manifold is recondensed into the storage vessel with liquid nitrogen. The measured volume of thionyl fluoride is condensed into the shielded 300-ml. Monel pressure reactor, which is attached to the vacuum line at F. The reactor is then closed and kept at —196°. 

A 100-mL HokeJ spun Monel vessel (rated for 5000 psi) prepassivated with either P2 or CIP and equipped with a Whitey stainless steel valve (SSD 1RM4) (Seattle Valve ) is loaded with 15 mmol (1.83 g) of Cr02p2 (by PVT techniques) using a well-constructed Monel or nickel metal vacuum line (prepassivated with CIF) and equipped with Whitey valves and Swagelok connections at - 196° (liquid N2). An excess of fluorine (Mathesoiifll) (120 mmol) is introduced into the Monel vessel by a pressure difference... 

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