March 27, 1951 PRESCOTT, JR MULTIPLE CHISEL STRUCTURE FOR DISINTEGRATING AND REMOWING2,546,700 INCRUSTATIONS FROM INTERIOR WALLS OF RECEPTACLES Original Filled Sept. 2, 1944 2. Sheets-Sheet

INVENTOR. 6A74azas/7 A2asco 77/2, 2 ATTORNEY. March 27, 1951 c. H. PREscoTT, JR 2,546,700 MULTIPLE CHISEL STRUCTURE FOR DISINTEGRATING AND REMOWING INCRUSTATIONS FROM INTERIOR WALLS OF RECEPTACLES Original Filled Sept. 2, l944 2. Sheets-Sheet 2

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Ave. 7 INVENTOR. Gaezais /7. A2a56O77. /e. BY ATTORNEY. Patented Mar. 27, 1951 2,546,700

UNITED STATES PATENT OFFICE 2,546,700 MULTIPLE CHISEL STRUCTURE FOR DIS INTEGRATING AND REMOVING INCRUS TATIONS FROM INTERIOR, WALLS OF RECEPTACLES Charles H. Prescott, Jr., Berkeley, Calif., assignor to the United States of America as represented by the United States Atomic Energy Commis sion Original application September 2, 1944, Serial No. 552,556. Divided and this application Novem ber 2, 1945, Serial No. 626,388 4 Claims. (CI, 15-104.16) This invention relates to apparatus for use in aging the hygroscopic compound com connection with packaging and/or closing, in the prises a subliming chamber, a condensing cham absence of air, receptacles containing material ber joined thereto, a storage receptacle and a that is rapidly decomposed or otherwise affected conduit connecting the condensing chamber and deleteriously when exposed to atmospheric con storage receptacle, means for maintaining a vacu ditions. More particularly, it appertains to cer um in the apparatus, means for heating the Sub tain implements useful in connection with vacu liming chamber whereby the uranium compound um apparatus adapted for the purification of is sublimed into the condensing chamber Where cheminical compounds such as uranium it is condensed, means for moving the Sublimed that must be handled in the absence, or substan 10 and condensed uranium compound into the con tial absence, of air. This application is a division duit and the storage receptacle, and means for of my prior copending application Serial No. hermetically sealing the charged storage recep 552,556, filed September 2, 1944, and contains tacle. The present application is concerned more claims directed to certain adjuvant apparatus particularly with certain adjuvant apparatus ele elements that have proved to be particularly 15 ments that have been found to be particularly useful in conjunction with the method and ap well adapted for assisting in maintaining the paratus forming the subject matter of the prior proper movement of Solid material, comprising application. the uranium or other compound, through the The invention has for an object the provision apparatus, and particularly through the sublim of adjuvant apparatus elements useful in con 20 ing and/or condensing chamber. nection with the vacuum packaging of a hygro It has been found that under the thermal con Scopic material such as hygroscopic uranium ditions obtaining in the subliming and/or con compounds. Other objects are to provide certain densing chambers, the uranium or other con apparatus elements useful in conjunction with pound forming the charge material and/or the apparatus for purifying and packaging uranium 25 uranium or other compound forming the Sub compounds under vacuuin conditions, and to seal lined and purified product frequently tends to hernetically vacuum containers charged with adhere tightly to the wall of the subliming uranium compounds. Additional objects are to and/or condensing chambers. Moreover, the provide certain apparatus elements useful in uranium or other compound, particularly that conjunction with apparatus adapted to isolate a 30 comprising the purified product, is sometimes uranium in a vacuum, to sublime a present in the apparatus in the form of lumps uranium chloride in a vacuum, to purify a ura or granules and/or conglomerated masses that nium chloride in a vacuum, and to store a ura require to be broken up if the broad objects of nium chloride in a vacuum. A general advance the apparatus are to be attained in the most in the art and other objects that will appear 35 preferred manner. Furthermore, it appears that hereinafter are also contemplated. the charge material itself that is introduced into In accordance with this invention, an appa the subliming chamber sometimes tends to con ratuS has been originated for packaging a vola glomerate, due to the thermal conditions obtain tile, hygroScopic compound, such as a volatile, ing within the subliming chamber and/or poS hygroscopic uranium compound, comprising sub 40 sibly in some cases due in part to a slight residual liming a hygroscopic uranium compound, con moisture content in the charge material. densing the Sublimed compound, charging a con Accordingly, certain adjuvant apparatus ele tainer with the sublimed compound, and her ments have been fabricated particularly with a Inetically sealing the container, all of the opera view toward the more efficient handling of the tions being conducted without exposing the hy 45 material undergoing processing in the Subliming groscopic uranium compound to the atmosphere. and/or condensing chamber of the receptacle Uranium coin pounds that are Suitable for treat charging apparatus forming the subject matter ment in this manner are uranium hexachloride, of the above-mentioned copending application , and the like. Serial No. 552,556. As will appear more fully An apparatus suitable for purifying and pack SO hereinafter, these adjuvant apparatus elements 2,546,700 3 4. are materials-handling elements so arranged and has two downwardly extending delivery ducts or employed in connection with the apparatus that tubes 34 and 38. The sublimed and purified ma they are operable from outside the apparatus terial is transmitted to a storage receptacle 38 through appropriate Wilson seals, thereby per through the tube 38, and unsublimed material is mitting them to be operated at will from without 5 moved through the tube 34 to a receptacle 40 the apparatus at the convenience of the operator, connected thereto at 62. The container 30 also without at the same time making it necessary has tubular extensions 44, i. 6 and 48 constituting to break the relatively high vacuum that is main portals for the devices that manipulate materials stained in the interior of the apparatus. being processed, as well as two ducts 58 and 52, HoW the foregoing objects and related ends it) located exteriorly of the path of material as it is are accomplished will be apparent from the foll proceSSed, for connections to apparatus capable lowing description including the principle, the of producing a vacuum of at least 104 mm. Hg. organization and various embodiments of the in A gaStight joint 5 is provided to facilitate assen vention, and the best node contemplated for bling and cleaning the apparatus. carrying out the same. This: description is am Near its center the horizontally disposed con plified by the accompanying drawings, in Which: tainer 3 has a Subliming Zone Surrounded by a Figure 1 is a fragmentary side VieW, in eleva furnace 33. his furnace consists of two Semi tion, of the combined charge purifying and re cylindrical electical resistance heaterS 58 and 60, ceptacle filling and sealing apparatus embodying capable of raising the mass of material being the features of the invention. 20 proceSSed to its volatilization and/or decomposi Fig. 2 is a fragmentary view, in plan, of the tion temperature. The temperature commonly end of the material moving device employed in empioyed in Subliming uranium hexachloride in the condensing end of the apparatus of Fig. 1. this apparatus is about 150° to 180° C., or even Fig. 3 is a side view, in elevation, Of the de as high as 210° C. The heaters have individual vice of Fig. 2. electrical connections 62 and 84 for a source of Fig. 4 is an end view, in elevation, of the device heating current. The heater Sections are con of Fig. 2. - structed to provide space for a thermocouple well Fig. 5 is a fragmentary view, in plan, of the 66. The thermocouple therein (not shown) is end of the material moving device employed in connected by conductors 68 and it to an indicat the feeder end of the apparatus of Fig. 1. ing and/or recording instrument 2, such as a Fig. 6 is a side view, in elevation, of the device potentiometer or voltmeter, which may be suit of Fig. 5. ably calibrated to indicate and/or record directly Fig. 7 is an end view, in elevation, of the de in terms of the tenperature prevailing Within the vice of Fig. 5. Subliming Zone. Fig. 8 is an enlarged fragmentary view, partly 35 For moving material inside the vessel 38 at the in section, of a portion of the apparatus of Fig. feeder end thereof, an implement comprising a l, illustrating the closing hood and a storage rod 4 carrying a chisel 76 and a hoe 3 is pro receptacle secured thereto, as Well as a typical Wided, to insure adequate rigidity, this rod Wilson seal arrangement by which the material should be about one-quarter inch in diameter. moving devices may be manipulated from with 40 The rod 4 extends through a conventional Wil Out the apparatus Without at the same time Son Seal 85 in the tubular extension 44, and breaking the vacuum existing within. carries On its external end a handwheel 82 by Referring now to FigS. 1 to 8 of the drawings, which the implement is manipulated. The chisel there is illustrated a purifying and packaging 76 and hoe 78 are ordinarily made of stainless apparatus constructed largely of glass and con Steel. The hoe is preferably in the form of an prising a hopper in which the material to be approximately 120 helical sector, tilted at an processed is placed before the purification opera angle of about 22.5 to a plane normal to the tion is started. A hopper having a capacity of axis of the rod, so that by rotating the rod is the about one liter is suitable. This hopper has a hoe can be screwed into the mass of granular conduit 2 through which it is filled with raw . 50 material in the chamber without pushing the en material, a tubular extension 4 designed to re tire maSS of material forward, thus breaking up ceive a conventional Wilson seal 6 having a lumps or aggregates of the material. - vacuum testing connection tube 3, and a duct For testing the gastightness of the connection 20 for connection to a vacuum-producing appara around the rod 74, the Wilson seal 80 has, as is tuS (not shown). A removable plug 22 fitting usual with these devices, a lateral tube 84 for tightly in the conduit 2 seals, this part of the connection to vacuujin-producing apparatus. . . apparatuS against the atmosphere. At the delivery end of the container 30, in the Raw material is released from the hopper 0 tubular extension 66, there is another material as desired by means of a feeding device compris manipulating arrangement comprising a rod 86 ing a stainless steel disk-like gate 24. This gate, 60 carrying a chisel 88 and a scraper blade 90, a comprising two slightly Warped semicircular metal surface of which is substantially normal to the sheets, is carried on a rod 26 that extends through axis of the rod. As clearly shown in Figs. 1 to 4, the Wilson Seal 6 and is operated by a hand the chisel portion 88 comprises one chisel surface Wheel 28. A cylindrical rod made of one-quarter 92 adapted to contact more or less closely the inch stainless or ordinary carbon steel stock is 65 wall surface of the chamber 36 in order to scrape Suitable. Rotation of the handwheel 28 produces sublimate therefrom, and a second chisel surface rotation of the gate 24 which thereupon functions 3& extending ahead of, and substantially at right like a feed screw to release material from the angles to, the first-mentioned chisel surface 92, hopper in a conventional manner. thereby functioning to split portions of the sub The hopper le is connected to a sublining con 70 limate away from the main bulk thereof before tainer or kiln 30 by means of a duct 32, through the first-mentioned chisel surface 92 can develop which the raw material is delivered by gravity a Wedge action upon the main mass of Sublimate when released by the gate 24. Ordinarily, the when the tool is driven in a direction generally container 30 is a 2.25, inch diameter Pyrex glass parallel to the Wall Surface. It will also be cylinder about 50 inches long. The container 30 75 noted that the second-mentioned chisel surface 2,546,700 5 6. 94 slopes with respect to the axis of the rod, The conventional Wilson Seal 44 that closes forming a relatively sharp trihedral angle at the the tubular extension 40 is typical of the con Outermost point, which point (as shown in Fig. 3) wentional Wilson Seals that have been referred lies somewhat below the plane of the first-men to hereinbefore, and consequently will be de tioned chisel surface 92, the whole thereby form 5 Scribed in Some detail for the sake of complete ing an extremely effective chisel. neSS. This Seal comprises a plug portion 60 The rod 86 extends through an improved Wil having a seat upon which a rubber diaphragm 62 son Seal 96 and carries, exteriorly of the con is Supported. A circular and annular spacer 64 tainer 30, a handwheel 98 by which it is manip engages the diaphragm S2 and, in turn, is en ulated. This rod is also preferably of One O gaged by a Second rubber diaphragm 66. This quarter inch round stock. The diaphragm case aSsembly is maintained in position by a Washer or holder of the Wilson seal carries the custon 68 and a screw plug . A vent 2 in the ary vacuum connection tube foo. annular portion of the spacer 64 connects the The improved Wilson seal 96 preferably em Space between the rubber diaphragms 62 and ployed in conjunction with rod 86 is of a new 5 66 to a tube. E 6. This tube 74 is employed design, being specially constructed to allow more as a vacuuin Connection for testing the ade than the usual (12) defection for the rod 86, as quacy of the Seal made between the rod 42 and is customary in the conventional Wilson Seal, the two cooperating diaphragms 62 and 66. such as seal 80. This improved Wilson Sea is By evacuating the tube 74, it is possible to de fully described in U. S. Patent 2,442,622 to Starr, 20 termine before the processing of naterial is issued June 1, 1948. For specific details of this Started whether or not a gastight seal between improved Wilson seal reference may be had to the rod 42 and the plug 6 is formed by either the aforementioned Starr patent, it being suf or both of the diaphragms 62 and 66. ficient for present purposes to note in passing. The receptacle 38 is cylindrical in shape and that the greater range in movement afforded by 25 has a circular mouth 8C in the top. Surround this seal is obtained by an arrangement includ ing the mouth is a groove 82 designed to re ing a swivel joint. This joint, located between ceive the depending skirt or fange 84 of the the case carrying the diaphragms (not shown) cap 50, and a groove 86 for packing purposes. and the plug fitting into the extension 46, is coV Ordinarily, the mouth 80 and grooves 82 and ered by a conventional flexible thin metal bellows 30 86 are located concentrically in the top of the f2. This bellows is soldered to the aforemen receptacle. An annular gasket 88, preferably tioned parts to permit maintaining the high made of rubber, is positioned in the groove 86 vacuum inside the apparatuS. in Order to piroduce a vacuum-tight Seal between The tubular extension 48 extending upwardly the receptacle 38 and the hood 3. Preferably, from the container 3 carries a conventional 35 the receptacle 38 is made of stainless Steel, for Wilson seal to 4, incorporating a vacuum testing example, 8–8 (18-Cr, 8-Ni; U. S. S. #316) stock, connection tube 6. A rod 8, which extends but other metais not readily attacked by the through the Wilson seal. O4, has a pointed and/or Vapors of uranium halides may be used if desired. notched end O and carries adjacent thereto a The receptacle 38 is secured to the hood 30 small hook 2 pointing in substantially the op While being filled and closed by a cage-like frame posite direction. This rod is conveniently made 20. This frame comprises a split ring that from one-eighth inch round stock. A handwheel grips the receptacle 38 and a split collar that 4 at the external end of the rod 08 is utilized extends over the fange 38 on the hood 39. for imparting movement thereto. The split ring is indicated by the reference nu Referring now to Fig. 8, the duct 36 projects 45 neral 22 and the Split collar by the reference into a hood 3C and terminates in a nozzle 32 numeral 24. The split ring is held in gripping which is surrounded by a telescoping spout 34. engagement with the receptacle 38 in a manner During the time the storage receptacle 38 in be that Will be apparent upon inspection of FigS. ing filled, this spout projects into the mouth of 1 and 8, and is is turn Secured to the Split collar the receptacle and is supported on the top of the 50 264 that supports the entire assembly in receptacle by an integral, laterally projecting tight relation against the flange 38 of the hood flange 36. This arrangement forms a continu 30 in a manner that likewise will be apparent ous passage, whereby material falling through upon inspection of these figures. A flat ring 206, the duct. 36 is conducted into the interior of the preferably made of rubber, serves as a cushion receptacle, thereby avoiding an accumulation of 55 between the Spiit collar 24 of the frame 299 material in fine particle or dust form on the top and the frangible flange 38 of the hood 30. of the receptacle adjacent the closure, which Further Specific details of this assembly are not accumulation of material would interfere with pertinent to the present claimed invention, but sealing the closure. -, may be obtained by consulting the above-men The hood 30 comprises a flange 38 conform 60 tioned prior copending application Serial No. ing to the top of the receptacle 38 and a laterally 552,556. extending tubular portion 40 that forms the The cap 50 that is adapted to be Solidered into housing for a rod 42 that is supported within sealing engagement over the mouth of the re a conventional Wilson seal 44. This rod, pref ceptacle 38 constitutes an arrangement that is erably of one-quarter inch round stock, is manip 5 fully described in the Copending application of ulated by a handwheel 46 and carries on its Duane C. Sewell, Serial No. 554,926, filed Sep inner end a hook 48 which, during the receptacle tember 20, 1944, while the method of completing filling operation, Supports a cap 50 for the re the appropriate Seal between the two is fully ceptacle 38 in a position within the lateral ex described in the above-mentioned prior copend tension 40 where the cap cannot interfere With O ing application Serial No. 552,556. Since this the descent of material into the storage recepta subject matter forms no part of the present cle (Fig. 1 position). The hook 2 on the rod Cained invention, it is deemed unnecessary to 08 Supports the telesconic spout 34 above the describe it in detail at this point, it being sufi mouth of the receptacle 38 during the receptacle cient to note in passing that the cap 50 re capping Operation (Fig. 8 position). 5 movably Supports an electric heater 20, the 2,546,700 7. 8 heater 20 being Secured in place by an arrange lying between the heater 56 and the duct 48 ment including a screw 22 threaded into the functions as an air-cooled condenser; it may cap 50. The heater includes an electric resist be additionally noted that, when and if desired, ance element, one terminal of which is grounded Supplemental cooling structure, Such as a Sur to the cap 56 and the other terminal of Which rounding coil (not shown) through Which is cir is connected to a terminai post 24 in the form culated a cooling medium. Such as Water, may of a loop or eyelet. The circuit for the heater be provided at this point. element may be completed (in a manner not The condensate of uranium hexachloride shown) by Setting the notched end ii of the usually begins to appear When the charge has rod 8 against the loop 2 fil, and by connecting reached a temperature of approximately 80° C. the rod (38 and the receptacle 38 to a suitable However, temperatures. Somewhat in excess of current Source by a circuit having a Suitable 150° C., for example in the range of approxi Switch (not shown) for making and breaking mately 150 to 190° C., are preferred for the the heater circuit. Sublimation of this material at a practicable rate. Considering now the mode of operation of the 5 The Sublimation of the UCls may be carried to apparatus shown in FigS. i to 8, the hopper Substantial completion by raising the tempera is filled with a mass of raw or crude hygroscopic ture to about 210° C. for a short time (up to material 32G (such as uranium hexachloride) about thirty minutes) at the end of a run at in Subdivided form through the conduit 2, and the lower temperature mentioned. The use. of the plug 22 is fitted into the end of the con 20 the higher temperature for extended periods is duit f2 in gastight relation. A quantity of glass Ordinarily not desired because uranium hexa or other relatively inert material 302, in the chloride begins to decompose slightly at 100° form of powder or Small beads, is placed in the C., and at an appreciable rate above. 150° C. in container 30 in a position from which it can be WaCLO. later advanced toward the Sublining Zone for 25 The layer of glass 306 Serves to retard or a purpose to be noted more fully hereinafter; prevent the fiOW of Wolatilized uranium con a previously prepared receptacle cap 5i is Sus pound in the opposite direction. When the va pended upon the hook 48 carried by the rod porization of the charge has been completed, the 42 in the tubular extension 48; a previously glass and residual matter from the charge is prepared storage receptacle 38 is secured and 30 raked back and into the receptacle 40 as shown sealed to the hood 30 by the frame 29), the at 310, except for a portion which preferably is telescopic Spout 34 being adjusted in the mouth retained in the tube 30 between ducts 32 and f 80 of the storage receptacle 38; he receptacle 3 to serve as a vapor blocking layer for the i) is secured to the tube 34; and the joints 2 Succeeding mass of crude material to be proc and 54 are closed, Preferably, the joints 42 and 35 essed. Another portion of the crude material 54, as well as the connections between the con 3 is then admitted to the tube 30 from the duit 2 and the plug 22 are sealed in a gastight hopper 9 and is positioned in the heating zone manner with ordinary sealing wax. Similarly, at 34, after which it is covered with a layer the connection between the tubular extension 306 of Subdivided glass and nonvaporized ma 4 and the Wilson seal 6, the connection between A) terial from a previous run or runs, and another the tubular extension A4 and the Wilson Seal 83, Vaporization cycle is conducted. These cycles the connection between the tubular extension are then repeated without breaking vacuum until 46 and the Wilson seal 96, the connection be the supply of crude uranium hexachloride 300 tween the tubular extension 8 and the Wilson has been exhausted. seal 04, and the connection between the tubular 45 The condensed uranium hexachloride 308 that extension 49 and the Wilson Seal $4 are also collects on the cooler portions of the wall of the sealed with sealing wax. The vacuum-testing container 30 is chiseled away, preferably after tubes 8, 8.4, 30, 6 and 74, respectively as each sublimation, With the chisel 88 and raked sociated with the Wilson seals 6, 8), 36, - 4 into the duct 3. With the hoe 9. The sublimate and 44 are Suitably connected to the Vacuum 50 is deposited on the inside of the tube 30 in a zone producing apparatus and the several Wilson ordinarily extending from about one-half inch seals are tested in order to insure that the ap to twelve inches from the edge of the hot Zone, paratus as a whole is gastight. The ducts 28, with the thickest deposit usually occurring in 53 and 52 are then connected to the Vacuum the first three inches. The uranium hexachloride producing apparatus, whereby the container 39 55 that Sublines below 170° C. condenses in this and the connected parts are evacuated to a rela three-inch zone in a layer usually about 3%-inch tively low pressure, such for example as 10 thick. This deposit has a mechanical strength ill. Hg. - . . approximately equal to that of anthracite coal A portion of the crude uranium hexachloride and hence must be chiseled off the wall. HOW 30g is introduced into the container 38 by suit 60 ever, the adhesion between the deposit and the ably rotating or reciprocating the handwheel 28 glass is . Somewhat weaker than its ...internal in order to control the gate 24, and is positioned strength or cohesion, so that the deposit. tends to in the heating zone within the furnace, as shown scale or break off in large pieces, particularly at 334, by means of the hoe 8. Thereafter tha when the wall surface of the container 30 is clean. subdivided glass or other relatively inert ma 65 For this reason it will be apparent that the terial 302 is spread over the adjacent or feed chisel 88 comprising the forward cutting edge side of the pile of crude uranium hexachloride, 94, tending to break off the deposit in the form as shown at 36, thereby preventing or substan of smaller pieces before large pieces scale off tially preventing the flow of vapors toward the the container wall, is of particular advantage. in feed side of the apparatus. Heat is then ap 70 handling material of this character. Pieces too plied, causing volatilization of the uranium hexa large to pass through the duct 36 may be chopped chloride, the vapor of which flows toward the into smaller pieces by means of the pointed end cooler portion of the container 3) and con of the rod 98. denses thereon, as shown at 308. Accordingly, Although by this method all of the sublimed 'it will be noted that the portion of the container and purified uranium hexachloride may not be 2,546,700 10. completely removed from the wall of the con cooler portions of the tube 30 is ordinarily first tainer 30, and although some slight amount of observed at a temperature of about 365 to 380 uranium hexachloride vapor may have seeped C., under the pressure conditions already set through the barrier layer 306 and deposited in forth. However, temperatures of from approxi Solid form in the feed end of the tube 39, it is un mately 500 to 550° C. or higher are required for necessary to clean the tube after each run Since the Sublimation of this material at a practicable. dry air (which may be introduced into the ap rate. When these higher temperatures are em paratus when fresh feed material is introduced ployed it may be desirable to employ additional into the hopper 0 and which might remain in Support for the tube 3 to prevent any sagging extremely small amount in the apparatus) causes O of the tube due to the higher temperatures neces no visibie decomposition of the uranium hexa sary for the Sublinnation of uranium tetrachlo chloride. It is therefore customary practice to ride at practicable rates. clean the entire apparatus only after a number It will be understood that when a sufficient Of runs. -- quantity of Sublinate of highly purified uranium A single run of the type described above usual hexachloride (or of highly purified uranium ly requires a full working day and produces ap tetrachioride, when the starting material 308 com proximately one-half kilogram of highly purified prises more or less inpure uranium tetrachloride uranium hexachloride, these figures being ex as described in the preceding paragraph) has emplary and based upon the particular apparatus been deposited on the walls of the container 30. chOSen by Way of illustration...... as shown at 308, the deposit is removed from the Instead of treating an impure uranium hexa Walls, broken into sufficiently Simall particles to chloride to obtain the desired highly purified pass through duct 36, and scraped into the duct uranium hexachloride product as described above, by Suitable manipulation through the correspond uranium pentachloride may be employed as the ing seals of rod 83 carrying scraper 90 and chisel starting material for the production of uranium 25 88 and rod 8 having the pointed end G. In hexachloride by the reaction mechanism dis this manner sufficient purified sublimate is col closed in the copending application of Francis A. lectCd to fill the storage receptacle 38 to the de Jenkins, Serial No. 494,447, filed July 13, 1943; sired level. Where two or more sublimation cycles i.e., by the disproportionation of uranium penta are required to obtain the desired quantity of sub chloride into uranium hexachloride and uranium Si limate, care is taken to maintain the vacuum tetrachloride under the influence of heat. When in the System between successive cycles, as pre uranium pentachloride is used as the starting viously mentioned. r material 300, it is heated in the subliming zone to Having collected the desired quantity of puri a temperature ranging from about 80° to about fied sublimate in the storage receptacle 38, the 180° C. but preferably toward the upper end of rod 98 is manipulated so that hook ff2 lifts the this range. Temperature as high as 250° C. may telescopic spout 34 from the filling position be employed for short periods, so as not to cause shown in Fig. 1 to the capping position shown in undue decomposition of the produced uranium Fig. 8, the rod 42 with its hook 48 carrying the hexachloride. At such temperatures, and under cover 56 is manipulated to move the cover from high vacuum, the uranium pentachloride is de its retracted filling position shown in Fig.1 to the composed into uranium tetrachloride and ura position shown in Fig. 8, and the cover is there nium hexachloride, the latter passing out of the upon placed in capping position with its skirt heated zone in the form of vapor which is con (84 disposed in groove f82 of the receptacle 38. densed in the cooler portion of the container 30 (It will be understood that the groove f82 in from Which it is removed and loaded into the the top of the storage receptacle 38 and the skirt storage receptacle 38, as more fully described * 84 of the cap iSC will have been prepared pre above. A residue, mainly uranium tetrachloride, viously for the soldering operation, in the manner of Over 50 per cent of the original material is left fully described in the prior copending applica in the sublimation zone. As this residue ac tion Serial No. 552,556). Rod 42 is then ma cumulates in the sublimation zone during and as 50 nipulated So that its hook 48 supports the tele a result of the disproportionation of successive Scoping spout 34, thereby freeing rod 08 with charges of uranium pentachloride and the at its pointed end. for another purpose, namely, tendant vaporization of uranium hexachloride that of completing the electric circuit to the re produced thereby, the undesired accumulation of ceptacle cap heater 2 . For this purpose the residue is raked into the duct 34 and collected in the receiver 40 at desired intervals for suitable rod O8 is manipulated so that its notched end O salvage operations, preferably however retaining bears firmly upon the eyelet 24 that forms a each time sufficient of hite residue in the con terminal post for the resistance element of the tainer 30 to serve as a blocking layer 36 for the heater 2 that is attached to the cover 50. Succeeding charge of uranium pentachloride that Upon completing the electrical circuit including is positioned in the subliming zone at 304. 60 the heater 2f ), the latter is energized and there ... Uranium tetrachloride of more or less impure by Supplies sufficient heat to the cap 50 to melt a form may also be used as the starting material mass of Solder, such as Wood's metal, that is em 300 where it is desired to prepare and/or pack ployed to hermetically seal the cap 50 to the re age this compound in a highly purified form for ceptacle 38. The circuit is then opened and, after subsequent use. In this case the operation of 65 Cooling, the Wood's metal forms a hermetic seal the apparatus is generally similar to that already between the skirt 84 of the cover 5 and the described for the case of uranium hexachloride, top of the storage receptacle 38. The frame 200 except that considerably higher temperatures, by which the receptacle 38 is clamped against the such as 512 to 520° C., are preferably employed 70 flange 38 of the hood 3e may then be unfas for. Subliming the uranium tetrachloride since tened, and the storage receptacle 38 with its her this compound is considerably less volatile than metically sealed contents removed from the ap uranium hexachloride. In general, a temperature paratus. Another receptacle cover or cap 50 of at least 500° C. is preferably employed. Con and another storage receptacle 38 (previously pre densation of purified uranium tetrachloride in the 75 pared for the soldering operation) may then be 2,546,706 1. 2 placed in position in the apparatus, and the ingahead thereof while sloping rearwardly tiered purifying and sealing operations resumed. from, the cutting edges of the second-metationed The vacuum-producing device associated with cirisersloping with respect to the axis of the rod, the purifying and packaging, apparatus of Figs. 1 and forming a relatively sharp. trihedral angle to. 8 has not been shown in detail Since. it will 5 at the outermost point thereof, whereby portions: be understood that it may be purely conven of the material may be split away from the 5talk. tional in nature. Thus, this device preferably thereof by the second-mentioned chisel before. comprises two, liquid air traps and a mercury dif the first-mentioned chisel can develop a wedge. fusion pump. In addition, it is preferable to in action when the tool is driven in a direction. clude drying tubes provided with magnesium per O generally parallel to the wall surface. - chlorate and phosphorus pentoxide to dry the 2. In combination with a processing eha-Erbee. stream of air entering the apparatus when it islet in which material is adapted to be proeessed downto atmospheric pressure. substantially out of contact with the atmosphere; When processing corrosive materialis Such as a seal in a wall of the processing chamber, and are described herein, it is desirable-particularly 5 a rod extending through the Seal in a Susstan in view of the relatively elevated temperatures tially gastight manner, the end of the rod withs enployed to use specially selected materials of in the processing chamber, constituting airli, edged cCInstruction for the apparatus. Because of its tool designed to remove from the-wall of the: heat resistance, Pyrex glass is the preferred ma processing chamber a material tenaciously ad terial for constructing the principal parts of 20 hering thereto, the edged tige comprising at the apparatus. The rods 26,74, 86, fo8 and 42, chisel adapted to rest upon the wall surface-to the hoes 8- and 98, the hooks - f2 and 48, and scrape the naterial therefrom, and a second the storage receptacle 38-are preferably made of chisei substantially at right angles' to the first stainless steel stock, such as 18-8 (Cr-18, Ni-8; mentioned chisel and projeeting ahead-tiereof ti; S. S. #316), in order to resist corrosion by 25. While sloping rearwardly, therefrom, Wheresy. -containing materials inside the appa portions of the material may be split away from ratus. The chisels or spikes. T6 and 88 are made the bulk thereof befores: the first-inentioned of tool steel. The receptacle cap 50 may be chisel can develop a wedge action-when the tool. made of Soft iron, and, since soft iron is not is driven is a direction generally parallel to the easily wet by molten Wood's metal (the material 30 wall. Surface. ordinarily used for soldering the cap to the stor 3. In combination with a seal adapted for age receptacle), it is desirable that the skirt f84 location in a Walf of a processing chaniser in on the cap 50 be coated or tinned with a metal which material is adapted to be processed sub that is readily wet by such an alloy; for example, stantially out of contact with the atmosphere, a noble metal such as Silver, gold, platinum, an edged tool comprising a rod carrying a first iridium- or -osmium. For like reasons, it is pref - chisel adapted to-rest upon the wall surface to. erable also to coat, the interior of the groove -82. scrape the material therefrom, the cutting-edge with a layer of wetting metal, such as one of of the first-mentioned chisel being substantially the-noble metals just mentioned. The Wood's perpendicular to the axis of the rod, and a second metal referred to above- is... a. wery, low-melting. 40 chisel. Substantially at right angles to the firste. material, usually the quaternary. alloy. 50, Bi, mentioned chisel and projecting ahead thereof 25, Pb, 2.5i Sri aref 1:25, Cd. This substange nets: while sloping rearwardly therefrom, the cutting at 655. C. A. silver solder comprising 63. Ag., edge of the Secondmentioned chise sloping with 30. Cusand 7.5: Zris especially-suitable for tinning respect to the axis of the rod, and forming a ther skirt f84 on the cap 50. relatively sharp trihedral angle at the Outermost While, the foregoing apparatus as: been de point, thereof, whereby portions of the material. seribed in connection with a process-for-treating may be split away from the bulk thereof by the certaia named uranian compounds, it will be. second-mentioned chisel before the first-men obvious: that it is not limited to use. With such tioned chisel- can develop a Wedge action wher. raterials. It. Will be. especially obvious: that the 50 the tool is driven in a direction generally paralled adjuvant apparatuSelements to which the claims: to the wall surface. herein: are particularly directed are of wides ap 4. For use in the removal ficorn, the Wall of a plication, and that they will be found to be processing chamber of...material tenaciously...ada. well adapted: for processing other materials in hering thereto, chisel means comprising an elons. vacuo. Where it is necessary:tomove the laterials gated rod mounted...for rotatable...and reciprocable undergoing processing frogs without the appa movement, in a stationary wall of the chamber ratus, Without at...the same time. disturbing the and having; a unitary chisel block rigidly affixed Vacuum conditions withini. to: one end of Said, rod, a first chisel, surface...on. Erobably, many apparently widely different Said block extending frona one-side: thereof, and embodiments of this invention may be made 60 terminating forwardly in a straight edge-extendee Without... departing: from the principle breadth ing transversely of said rod, a. pair of converging and Spirit thereof and it is to be understood, chisel Surfaces: extending: from an opposite: side therefore, that... this; in Vention is not limited to of the block, and intersecting to figra as straight the Specific. embodiments, thereof, except, as en edge. Which projectS. from. Said opposite side compassed in the following claims. 65 What is, claimed is: diagonally acroSS the axis of the rod...ands ter. 1. An edged. tool designed to remove from the minates in a sharp point in forwardly spaced wall of a processing chamber a material tena relation to Said transversely extending straight ciously adhering thereto comprising a rod car edge- to provide an open space. in said block - rying a first chisel adapted to rest upon the wall O intermediate said first surface and said converg Surface to scrape the material therefrom, the ing Surfaces, and a pair of forwardly converge cutting edge of the first-mentioned chisel being ing surfaces defining a straight edge at the inner substantially perpendicular to the axis of the riost portion of said space, whereby material-first loosened by said second surface and later's re anglesrod, and to thea second first-mentioned chisel substantially chisel and atproject- right rs moved by said-first surfaeemay be passed through 2,546,700 13 14 said open space during longitudinal movement Number Name Date of the chisel means. 1,098,128 Schlacht ------May 26, 1914 CHARLES H. PRESCOTT, JR. 1,347,649 Mosher ------July 27, 1920 1,419,886 Muller ------June 13, 1922 REFERENCES CITED 5 2,246,421 Tate ------June 17, 1941 The following references are of record in the 2,322,419 Cranford ------June 22, 1943 file of this patent: 2,354,245 Corbosiero ------July 25, 1944 UNITED STATES PATENTS FOREIGN PATENTS Number Name Date in Number Country Date 267,306 Gall ------Nov. 7, 1882 8,525 Great Britain ------of 1884 343,769 Levi ------June 15, 1886