Valveless Shut-Off and Transfer Device

This invention relates to a liquid shut-off and transfer device and more particularly, to a device which contains no valve mechanism.

Often, it is important to minimize the internal volume of a gas transfer line. The transfer of a high pressure gas, usually at an elevated temperature, without the use of a valve is desirable. Valves or fittings, such as a "Tee" fitting generally have deadend portions. Gas being transferred is diluted with previous gas trapped in the dead end pockets.

Particularly in analytical measurements, such as gas chromatography, the elimination of such deadend pockets is important. Since the volume of gas being analytically measured is usually quite small, it is important to minimize the internal volume of the gas transfer line.

Solder and solder-like materials are well known. These are referred to herein as "eutectic" materials, meaning that they solidify below a critical temperature and liquify above a critical temperature, which critical temperature is within a range which can be easily controlled to selectively liquify or solidify the eutectic material. Fusible plugs of eutectic material are used in safety-related devices such as over temperature protection in gas cylinders, or to permit a flow of water into the sprinkler heads. These are "one shot" devices which cannot be reclosed.

It is an object of the present invention to provide a valveless transfer line which minimizes internal volume and has no "deadend" pockets.

It is another object of the present invention to use a eutectic material as the shut-off element in a transfer line.

The shut-off and transfer device of the present invention has a conduit with a loop which contains a eutectic material, i.e., solder or a solder-like material. The material solidifies below its critical temperature to block the loop and liquifies above its critical temperature to open the conduit to the passage of gas. A baffled enclosure between the loop and the outlet of the conduit contains baffles which retain the material in the loop when gas is passing through it. When the pressures at the inlet and the outlet of the conduit are equalized, the liquid material returns to the loop where it solidifies, thereby again shutting off the device. In accordance with the present invention, the internal volume of the transfer conduit is minimized. Also, the looped conduit has no deadend portions as generally found in valves or fittings so that gas being transferred is not diluted with any previous gas trapped in deadend pockets.

The shut-off and transfer device of the present invention has particular applicability to transferring gas from a shaker bomb, typically used to prepare mixtures of hydrocarbon oil and catalyst, to an analytical instrument such as a gas chromatograph. The transfer device of the present invention is easily attached to the shaker bomb in a manner which presents no problem during the heating and vigorous shaking to which the bomb is subjected during preparation of the mixture. Thereafter, the bomb is quenched with water to cool the bomb, stopping the reaction, and resolidifying the solder material in the loop. The capped end of the loop is unsecured from the bomb, the cap removed, and the free end is fitted with a baffle and a line to means for transferring the gas in the bomb to an analytical instrument, such as the gas chromatograph system. In this matter, small quantities of gas are reliably transferred from the shaker bomb to the gas chromatograph without contamination by other gases which might otherwise be trapped in the valves interconnecting the bomb with the analytical instrument.

The foregoing and other objects, features and advantages of the invention will be better understood from the following more detailed description and appended claims.

FIG. 1 shows the valveless shut-off and transfer device of the present invention;

FIG. 2 is a cross-section of the loop;

FIG. 3 is a cross-section of the baffled enclosure;

FIG. 4 shows the transfer device of the present invention attached to a shaker bomb during preparation of a catalyst and oil mixture; and

FIG. 5 shows the contents of the shaker bomb being transferred to a gas chromatograph by the transfer device of the present invention.

Referring to FIG. 1, the shut-off and transfer device of the present invention includes a conduit having an inlet 11 and an outlet 12. A loop 13 in the conduit contains a eutectic material which solidifies below its critical temperature to block the loop and liquidifies above its critical temperature to open the conduit to the passage of fluid, typically gas. A baffled enclosure 14 is between loop 13 and the outlet 12. The enclosure contains baffles which retain the eutectic material during the time that it is liquefied and gas is passing through the conduit. A similar baffle enclosure 15 may be provided on the inlet side, but is not necessary.

FIG. 2 shows a cross section of the conduit wherein the solder or the solder-like material 16 is solidified in the loop. A heater 17, or a furnace, provides means for controlling the temperature of the material above and below its critical temperature.

Tin-lead solders which have a melting temperature between 240.degree. F. to approximately 1,000.degree. F. are suitable for use. In the shaker bomb application, to be subsequently described, care must be taken to use a solder which will not contaminate the gas. For example, it has been found that some silver solders can catalytically change the composition of the gas to be analyzed. On the other hand, most tin-lead solders are sufficiently inert to be usable.

The looped conduit of the present invention can be made, for example, from 1/16 inch OD stainless steel tubing with a 0.020 inch ID, which has an internal volume of only 0.005 cc per inch of length. An even smaller tube of 0.010 inch OD by 0.004 ID has only 0.0002 cc/inch of length. Internal volume of the transfer line can be reduced even further by eliminating the baffle 15 on the high-pressure end because gas flow will be away from that end.

FIG. 3 shows a cross-section of the stainless steel baffled enclosure wherein baffle plates 18-21 retain the liquid during gas transfer.

Referring to FIG. 4, a shaker, or sample, bomb 22 is typically a sealed vessel of approximately 1,000 cc. In exemplary use, a mixture of catalyst and heavy oil is placed in the vessel which is sealed. The vessel is heated. Simultaneously, vigorous shaking, as by the reciprocating piston 23, is applied to the shaker bomb. The inlet end of the loop 24 is connected to the top outlet 25 of the shaker bomb. A cap 26 closes the other end. The transfer device of the present invention is securely fastened to the shaker bomb so that it can be subjected to its normal heat and violent shaking. After a designated reaction time at specified temperatures, generally 300.degree. F., to 1,000.degree. F., the bomb is quenched with water to cool it rapidly, thereby stopping the reaction of the contents. This also solidifies the eutectic material in the loop at 24.

After the bomb is quenched, the cap 26 is removed from the bomb and the free end is fitted with a baffled enclosure 27. A restrictor valve 28, or capillary restrictor, connects baffled enclosure 27 to the gas chromatograh 29.

While a particular embodiment of the invention has been shown and described, various modifications are within the true spirit and scope of the invention. The appended claims are, therefore, intended to cover all such modifications.