US1482684A - Sublimator - Google Patents

Description

J. HORTVET web 5, 1924;

SUBLIMATOR Filed Feb. 19, 1925 2 Shees-Sheet l Feb.. 5 1924..

J. HORTVET SUBLIMATOR Filed Feb. 19, 1923 2 Sheets-Sheet 2 Patented Fabi 5, llQt-lo v"narran stares 'natuur ortica susan/aaron Y application tiled February le, tutti. derlei No. 619,952.

To all 'whom it may concern:

Be it hewn that lf, demos lllloirrvnr, a citizen of the United States, residing lull/linneapolis, in the county of Hennepin and State oi Minnesota, have invented a new and useful Sublimator, ot which the following is a specitication. Y

The increased utility ci? the process of sublimation in laboratories coupled with the commercial possibilities thereoi.2 has been attended withthe need of practical apparatus for separating and purifying substances in large as well as in small quantities and for general quantitative and microscopic anal sis.

ly invention relates to improvements in sublimators, its object being to provide a simple and durable apparatus of this kind which is convenient and ecient in operation and readily adaptable to the various conditions niet in the diderent uses to which it may be put.

TWith the foregoing and other objects in view, which will appear in the following de scription, the invention resides in the novel combination and arrangement ot parts and in the details oi construction hereinafter described and claimed.

ln the drawings, Fig. 1 is a plan view or a laboratory device embodying my invention; Fig. 2 is a sectional view illustrating the heater, the same being taken as on the line 2 2 of Fig. 1; Fig. 3 is a sectional view taken on the line 3-3 of Fig. l, the lower ortion of the heater being broken awa g ig. 4 is a detail sectional view taken on t e line 4-4 of Fig. 3; Fig. 5 is a vertical sectional view in detail illustrating a portion oi the body section and the base section oi the sublimation vessel, also a capsule, stand therefor and microscopic slide employed for microsublimations and Fig. t is a plan view in detail of the stand or block to support vessels for-substances in the base section ot the sublimation vessel.

Referring to the drawings, it will be observed that my improvement includes a heater A and a sublimation vessel B, which is removably supported by the heater. rllhe to heater A includes a base 10 and a cylindrical jaclret 1l rising therefrom. Within the upper end of the jacket 11 is a heating drum a? the side wall thereofcomprising a sleeve 12, which is smaller in 'diameter than the gaclret 11 and arranged in axial alignment et with respect thereto; 'lln's sleeve 12 has anl outwardly extending annular shoulder 13 resting upon the upper edge of the jacket and supporting saidsleeve therein. An annular cover-plate 14. having a central vessel e@ receiving openin 15 therein forms the top ot the drum. his cover-plate caps the sleeve 12, its margin being turned downward over a depending annular iiange 16 on the shoulder 13, thence turned upward within es said liange to join the cover-plate with the sleeve structure and to torni a rib for the reception ot Aset screws 17, the inner ends ot which engage beneath a bead 18 at the upper edge ot the jacket 11. The bottom of io the drum consists oi? a cup-like tray 19 tting closely within the sleeve 12 and slidable vertically therein. This tray 19 is supported at various elevations within the sleeve 12 by means of hanger rods 20. These rods, secured at the lower ends to the sides of the tray 19, slide up and down within hollow posts 21 rising -Sironi the cover plate 1d, Said .posts being equipped with binding screws 22 to grip said rods 20 and the rods being g@ equipped with handles'23 for manipulating the saine in raising and lowering the tray 19. Rising from the cover-plate lei is a standard 24 having a vertically adjustable clip 25 thereon. rllhis clip slidablv grips a agg, thermometer 26 reaching downwar through a notch 27 in the cover-plate 14 and into a sand bath 28 in the tray 19. 'lhe jacket 11 has an opening 29 in the side thereof to receive a burner 30, which is removably seated e@ on the base 10 in position beneath the bottom ci the drum a.

'lhe sublimation vessel B is removably seated in the drum a as shown in Fig. 3, more or less of the lower portion of said veso5 sel being encased within said drum, as desired, upon appropriate manipulation ol the hanger rods 20. Said vessel includes a cylindrical body section h and a base section c. rIlhe body section has a dome-like top terieu 'minating in an'axial nipple 31, the lower end of said section being open and the side wall contracted slightly at its extremity to form a beveled annularshoulder 32. The base section c is a cup-like Structure having an annular lip 33 to fit snugly over the shoulder 32 of the body section b and seal the open end thereof. Said section c comprises a removable subliming cup for the reception of substances to be treated. Such substances are preferabl placed in a dish, as at 34, Fig. 3, a stan -35 being supplied to elevate the same, if necessary.

For purposes hereinafter explained, a di aphragm 36 of platinum gauze or other sultable material is removably placed u on supporting lugs 37 projecting'inwar 1y from the margin of the shoulder 32.- In some operations the diaphragm is omitted and a relatively tall capsule, as at 38, Fig. 5, is seated in a central bore 39 in the stand 35. Within the u per end of the bodysection b is an accumu ator consisting of an axially arranged bulb d. Inletand outlet conduits 4() and 41 communicating with said bulb at its'upper end reach upward through the top of the bod section b then turn outward in opposite irections. Said conduits form hangers for the bulbd, the inlet conduit 40 being extended downward axially of the bulb and terminating at a point near the bottom thereof (Fig. 3). The inlet conduit 40 is designed to be detachably connected with a supply pipe or hose (not shown) for a cooling Huid. while the outletconduit 41 is designed to be detachably connected with a suitable drain pipe or hose (not shown).

In use, a substance to be treated for the purpose of separating a 4purified material therefrom or for the purpose of quantitative analysis, is placed in a dish 34 in the subliming cup c. The diaphragm 36 is aplied to the body. section b, as shown in Fig. 3, and the dlsh elevated, if desired, by the use of the stand 35 to bring the rim of the dish into close proximity to the diahragm. The sublimation vessel B is seated 1n the drum @(Fig. 3), the subliming cup c being nested in the sand bath 28. The tray 19 is lowered from elevated receiving position to encase the desired portion of the vessel B in the drum a, the thermometer 26 being correspondingly adjusted. The inlet and outlet conduits 40 and 41 are connected with inlet and drain pipes, respectively, and the nipple 31 is connected with a tube leading to a vacuum pump or other suitable pressure reduction device, -said-tube, if desired, being threaded through the eye 42 in thesupport 24. After lighting the burner 30 and guided by readings of the thermometer 26, the user accurately adjusts said burner to accord with the work or experiment conducted.. The sublimed material accumulates on the lower portion of the bulb d, 155V any part of such material dislodged therefrom being caught u on the diaphragm 36. Upon completion of t e sublimating process, the pipes to the conduits 40 and 41 are disconnected and said conduits suitably plugged. The nipple 31 is also disconnected from the vacuumtube. The sublimation vessel B is then lifted from the heater and after cooling the cup c is detached from the body section b.. Said section is then invert- 'ed without the removal of the diaphragm,

\which falls loosely into the space between the bulb d and shell of the body portion b. By means of a suitable solvent, the deposit on the bulb is washed through the nipple 31 into a crystallizing receptacle, the dissolved sublimate being thereafter suitably treated to attain the desired ends. In thisv connection attention is invited to the fact that the nipple 31 serves not only as a conduit for the exhaustion of air from the sublimating vessel B, but also as a drain for sublimate washed from the sublimation chamber within the body section b.

For microsublimation, when only a very small quantityof sublimable material is probably present, the substance is placed in the narrow base portion of the subliming capsule 38 (Fig. 5), said capsule being seated in the bore 39 in the stand 35 within the cup c. A glass slide 43 initially placed so as to rest on lugs 37 in the body section b is lifted by and covers the capsule 38 when the cup c is applied to saidbody section. Said slide, being in proximity to the cooling bulb d, serves as an accumulator for material sublimed from the substance in said capsule. For such microsublimation, the tray 19 is adjusted to an elevation encasing the cup c and only a small portion of the body section b of the vessel B. The cooling fluid pipes are connected to the conduits 40 and 41 and the vacuum tube is connected with the nipple 31 as above explained. Sublimation being completed, the vessel B is removed from the heater A and, after cooling, the cup c is detached from the 'body portion b. The slide 43 then bein accessible, may be removed and the sub imate thereon examined under a microscope without the use of a cover-glass.

Changes in the s ecific form of my invention, as herein disc osed, may be made within the scope of what is claimed without departing from the s irit of my invention.

Having describe my invention, what I claim as new and desireto protect by Letters Patent is:

1. In a device of the class described, a vessel adapted to contain a substance in the bottom thereof to be treated, means for heating the lower portion of the vessel, said vessel having anv elevated opening therein for the 2liA 'exhaustion ot air therefrom and an accumulator within said vessel presentin a surface for the deposition of material sub imed from said substance under heat, within the vacuous interior of the vessel.'

2. ln a device of the class described, a vessel adapted to contain a substance in the bottom thereof to be treated, means for heating the lower portion of the vessel, said vessel having an opening'at the top thereof for the exhaustion of air therefrom, an` accumulator bulb spaced centrally within the upper portion of said vessel, said bulb supplying a surface for the deposition of material sublimed from said substance under heat, within the vacuous interior of the vessel, an inlet duct for a cooling Huid leading into 'said bulb and an outlet duct for said duid leadin from said bulb. A

3,I ln a evice of the class described, a vessel adapted to contain a substance to be treated in the bottom thereof and'formed with an elevated opening serving, in the normal position of the vessel, as an outlet for the exhaustion of air therefrom and, in the inved position of said vessel, as a drain, means for applying heat to the vessel and a cooled surface within the vessel for the de osition of material sublimed from sald substance.

t. ln a device of the class described, a vessel comprisingl an elongated body seetion and a cup-like base section removable therefrom, said base section being adapted to contain a substance to be treated, said body section having an opening in the top v thereof serving, in the normal position ot fio Vcased in said the vessel, as an outlet for the exhaustion of air therefrom and, in the inverted position of said body section, as a drain, a bulb spaced centrali in the bod section near the top thereof, in et and out et conduits communicating with said bulb through the walls of the body section and supportln the bulb within said section, the inlet con uit being extended centrally downward in the bulb vto discharge against the bottom thereof, the lower portion of the bulb supplying a surface for the deposition of material sublimed from said substance, and a drum for encasing the lower part of the vessel, said drum having a bottom supplying a rest for the vessel, said bottom being adjustable vertically to va the area ofthe vessel eng and a burner beneath the drum for heating the same.

5. A vessel comprisin a body section and a closely tting cup-like ase'section, the latter being removable from the former to be charged with substances and emptied of the residue thereof after treatment, said` body section having an openin therein for the exhaustion of air from sai vessel, means for heating the base section of said vessel and an accumulator within the body section supplying 'a surface for the deposition of ma- -terial sublimed from said substance.

ving and securing said bottom at various elevations to encase more or less .of the vessel within the drum, means for heating the drum, A-said vessel comprising an elongated shell adapted to contain a substance in the bottom thereofto be treated, said shell having an opening` therein for the exhaustion of air therefrom and an accumulator within the shell supplying a surface for the deposition of material sublimed from said substance, under heat, within the vacuous interior of said shell. A

7. ln a device of the class described, a

vessel having an outlet for connection with pressure `reduction means, said vessel being adapted to contain a substance in the bottom thereof to be treated, an accumulator elevated within the vessel and presenting a surtace for the deposition of material sublimed from said substance, means for cooling the accumulator and a heating drum adapted to encase more or less of the lower portion of said vessel. y Y 8. ln a device of the class described, a vessel having an outlet for connection with pressure reduction means, said vessel being adapted to contain a substance in the bottom thereof to be treated, an accumulator elevated within the vessel and presenting a surface for the deposition of material sublimed from said substance, means for cooling the accumulator, a heating drum, said vessel being removably seated in the drum, said drum being adjustable to vary the height at which the vessel is encased thereby.

9. lln a device of the class described, a sublimation vessel, a heating drum for the vessel including an upright sleeve, a tray forming the bottom of the drum and supplying a rest for said vessel, said tray being adjustable vertically in said sleeve, a coverplate capping the sleeve and formed with an opening therein to t aboutv the sides of the vessel and means for heating the drum.

10. ln a device of the class described, an

elongated sublimation vessel, a heater including an upright cylindrical jacket having an opening in the side thereof to receive a burner, a heating drum within the jacket and above said burner, said drum comprising an upright sleeve formin the sidewall of the drum, a cup-like tray s idable within ottom for supporting,

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the sleeve, said tray forming a vertically adjustable bottom for the drum and a rest for the vessel, and a cover-plate capping the sleeve and formed with an opening therein 5 to freely receive said vessel.

11. A vessel comprising a body section and a base section removably applicable thereto, the former having an onenine at the bottom thereof, said base section comprising a clo- 10 sure for sealing said opening and a receptacle to contain a substance to be treated, means for heating the base section and a jacketed cooling medium within the body section supplyin a surface for the deposition 'of materia sublimed from said sub- 15 stance.

In testimony whereof, I have signed my name to this specification.

JULIUs HoRTvET.

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