US3770405A - Method of fabricating laboratory glassware - Google Patents

Method of fabricating laboratory glassware Download PDF

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Publication number
US3770405A
US3770405A US00246966A US3770405DA US3770405A US 3770405 A US3770405 A US 3770405A US 00246966 A US00246966 A US 00246966A US 3770405D A US3770405D A US 3770405DA US 3770405 A US3770405 A US 3770405A
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US
United States
Prior art keywords
tubing
passageway
section
sections
tubing sections
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US00246966A
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English (en)
Inventor
Angelis W De
R Luthmann
C Meehan
M Smith
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Bayer Corp
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Technicon Instruments Corp
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Assigned to TECHNICON INSTRUMENTS CORPORATION reassignment TECHNICON INSTRUMENTS CORPORATION MERGER (SEE DOCUMENT FOR DETAILS). Assignors: REVGROUP PANTRY MIRROR CORP.
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/56Labware specially adapted for transferring fluids
    • B01L3/561Tubes; Conduits

Definitions

  • ABSTRACT A method of fabricating laboratory glassware to provide a relatively small, rugged article of monolithic form having one or more relatively small fluid passageways-therein which may be characterized as having the appearance of wormholes.
  • the method includes the step of preforming sacrificial tubing, sections of which may be socketed together, and socketing the tubing with tubular connectors on assembly, prior to encapsulating the assembly in glass material. The sacrificial tubing is removed after encapsulation.
  • These fittings have also included coils such as for the mixing therein of plural liquids or for the time delay of fluid flowing therein, the turns of which coils may be few or many depending on the extent of the mixing action required or depending on the extent of the time delay required in phasing of the flow through the coil,
  • ductwork may be miniaturized. While ductwork may be formed of exceedingly fine bore tubing, such as capillary tubing, this tubing is very subject to breakage as by impact with a foreign object or, more often, in the handling of fittings constructed of such capillary tubing. It is common practice to connect a fitting with a required section of flexible tubing by manually fitting a nipple-equipped section of tubing so that the nipple enters a bore of the fitting and forms a seal therewith.
  • the sacrificial element may be removed by an etching process.
  • the resultant product has a bore therethrough for the passage of fluid.
  • a bore is a simple one, not requiring an internal junction.
  • One object of the invention is to provide a method of fabricating laboratory glassware of monolithic form having one or more fluid passageways therein, provided with plural fluid connectors protrudingtherefrom and which have internal fluid junctions.
  • Another object is to provide a method of fabricating an article having a fluid passageway in a glass material, which article has tubular connectors of a different material in communication with the passageway and extending without the glass material, utilizing tubing and tubular connectors of material having a higher melting point than the aforementioned glass material and an expansion coefficient compatible therewith.
  • the method includes the step of preforming the tubing in accordance with a predetermined layout of passageway, with openings corresponding to the respective connections between the tubular connectors and the passageway; and assembling by socketing the preformed tubing with reference to the tubular connectors.
  • the method ineludes the further steps of encapsulating the assembly in the glass material so as to permit access to at least the other end portions of the tubular connectors, utilizing heat; and removing the tubing to leave the passage way formed in the glass material with fluid connections to the tubular connectors held captive in the glass material.
  • FIG. 1 is a perspective view of an article of laboratory glassware formed in accordance with the method of fabrication .of the invention
  • FIG. 2 is an exploded view on a smaller scale of the assembly of parts in a mold-useful in theperformance' DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
  • FIG. 1 a typical product of the method of fabrication embodying the invention, wherein a monolithic slab or block of glass is indicated at 10.
  • the block which is elongated, may have a relatively long length of approximately l inches or more or the block may have a length of 1% inches, for example.
  • the size of the block will be largely dependent on the number, complexity, length and arrangement of the fluid passageways of circular cross section formed therein having only glass wall surfaces.
  • FIG. 1 merely by way of example is a passageway 12 extending intermediate the ends of the block.
  • This passageway has a vertical component, as in a curl portion 14. Though not shown, such a curl could well occur in a spiral portion of the passageway 12 according to the method of the invention as will be readily apparent hereinafter.
  • the passageway 12 has an inlet and an outlet formed by nipples l6 and 18 respectively, having fluid connections to the passageway 12 and held captive in the glass material so as to protrude therefrom in the manner shown to provide suitable coupling elements for fluid connections to conduits not shown
  • the nipples 16, 18 constitute tubular connectors and these may be formed of a suitable inert metal such as platinum or they may be formed, for example, of sapphire material which, like platinum, has a higher melting point than glass and an expansion coefficient similar to that of glass.
  • a similar tubular connector 20 extends from a distance above the block, where it is exposed, to a point inside the block where it has a junction with the passageway 12. Also, there is shown extending through one side of the block a similar tubular connector 212.
  • tubular connectors and fluid passages 12 and 24 in the glass block are such that a stream of fluid, say a sample liquid, may be inletted through the tubular connector 16.
  • a second fluid stream may join the fluid stream in passageway 12 through the junction between the passageway 24 and the passageway 12, the second stream, which may be a stream of a reagent liquid, being inletted to the tubular connector 22 having an internal junction with the inlet end of the passageway 24.
  • a third fluid stream, say of another reagent may be inletted through the tubular connector to join the first and second fluid streams in the passageway 12, and these three liquid streams may be intermixed in the curl portion 14 of the passageway 12 before exit from the passageway 12 through the tubular connector 18.
  • FIGS. 2-5 illustrate articles which may be utilized in making the product of FIG. 1.
  • FlG. 2 there is illustrated a box-like mold having a lower section 26, an upper section 28 and a floating top 30.
  • the lower section 26 has 9 bottom and four upstanding'sides in the upper margin of three of which sides semicircular notches 32 are formed.
  • the upper mold section 28 has corresponding sidewalls and has a vertical opening therethrough defined by the side walls. Three walls of the upper section 28, corresponding to those having the notches 32 therein, are provided in their lower margins with similar notches 34, only two of these notches being shown.
  • the upper section 28 rests on the lower section 26 with the notches 34 in registry with the corresponding ones of the notches 32 when the mold is assembled.
  • the floating top 30 of the mold having a vertical hole 31 therethrough, is structured and dimensioned to fill only the upper portion of the vertical opening through the upper mold section 28 when the mold is assembled.
  • the mold sections 26, 28 and 30 may be formed conveniently of carbon for nonadherence with the glass material.
  • upper and lower plates 36, 38 are employed, these plates being preformed of a suitable glass material, such as borosilicate glass, to fit with slight clearance within the side walls-of the mold.
  • the upper plate 36 has a vertical hole40 drilled therethrough which on assembly of the parts in the mold snugly receives the tubular connector 20 extending therethrough and which also extends with clearance through the hole 31 formed in the mold top 30.
  • Preformed sacrificial tubing of circular cross section structured in accordance with a predetermined layout of the passageway 12 in the finished article of FIG. 1,
  • This tubing after forming, has a curl 43 in it corresponding to the curl portion 14 of the passageway 12.
  • This tubing having a thin wall structure, is sufficiently ductile to be bent into the desired shape but sufficiently rigid to retain its shaped configuration which may include a coil portion, for example, as previously indicated.
  • the tubing 42 has an outer diameter closely approximating the diameter of the passageway 12.
  • such tubing which may be formed of a metal alloy, is required to have a higher melting point than that of the glass material forming the I plates 36, 38 and have, in addition, an expansion coefficient compatible with such glass material.
  • a metal alloy including nickel, cobalt and iron and sold under the trademark Kovar may be used for this purpose.
  • the tubing sections 42 having open ends for fluid communication with the tubular connectos l6 and 18, respectively, has holes 44 (FIGS. 4 and 5) formed in the side wall structure thereof in the proper location for fluid communication with the tubular connectors 20 and 22, respectively.
  • the open ends of the tubing section 42 and the holes 44 of this section define sockets for the assembly of parts as will appear clearly hereinafter.
  • the holes 44 which may be drilled, are of a diameter closely approximating that of the inner diameter of the last-mentioned tubular connectors.
  • the tubing section 46 has an open end for a fluid outlet in communication with the hole 44 and an open inlet end for communication with the tubular connector 22.
  • the tubing section 46 is illustrated merely by way of example as having an elbowed configuration after the preforming step, but it is to be understood that if desired the tubing section may have a helical configuration to form a spiral liquid mixing passageway or have some other configuration in accordance with a predetermined layout of a passageway in the final product. Also, it will be obvious that the tubing section 46 may have fluid connections, not shown, in addition to those illustrated and described, if desired.
  • the fluid inlet end of the tubing section 46 defines a socket, the fluid outlet end of this section defining a part to be socketed, as will appear more fully hereinafter.
  • tubular connectors 16 and 18 are assembled to the tubing section 42 in like manner to the assembly of the tubular connector 22 with the inlet end of the tubing section 46 and hence description of the assembly of the latter will suffice.
  • the tubular connector 22 is provided with an internal extension 48 which is received in the aforementioned socket defined by the fluid inlet end of the tubing section 46.
  • this extension 48 is formed as a separable tubular part or mandrel which is slidingly received in the connector 22 to extend within the last-mentioned socket, the extension member 48 constituting an alignment pin which extends entirely through the connector 22 as shown in FIG. 3.
  • the ex tension 48 which may be formed of sacrificial tubing, has an outer diameter closely approximating the internal diameter of both the tubular connector'22 and the tubular section 46.
  • The-manner of assembling the tubing section 46 with the tubing section 42 is shown in FIG. 4 and includes an extension member 50, similar to the member 48 but of shorter length, formed of sacrificial tubing and extending into both the open fluid outlet end of the tubing section 46 and into the socket hole 44 provided in the tubing section 42.
  • the extension 50 bottoms against the cylindrical side wall structure of the tubing section 42 as shown in the last-mentioned view. Hence it will be understood that the tubing section 46 is socketed in the tubing section 42 on assembly of the parts.
  • the assembly of the tubular connector 20 with the tube section 42 is similar to that of the previously described assembly of the tubular connector 22 with the tubing section 46.
  • the tubular connector 20 having an extension member 52 therein similar, to the extension member 48 previously described, has the lower or outlet end thereof resting for support on the tubing section 42.
  • the tubular connector 20 abuts the tubing section 42 as does the previously described fluid outlet end of the tubing section 46. Because in forming both the fluid connections of FIGS. 4 and 5 an internal extension is received within a socket, the corresponding ends'of both the tubular connector 20 and the tube section 46 may be squarely cut, instead of being cut to conform to the circular cross section of the tubing section 42.
  • the extension member 52 bottoms against the circular cross section of the tube section 42 and the extension member 52 extends without thenipple 20 as shown in FIG. 2.
  • this assembly may be placed in the lower mold section 26 with the lower glass plate 36 below the assembly and supported on the bottom of the mold section.
  • the aforementioned tubular connectors 16, 18 and 22 are supported within corresponding ones of the notches 32 formed in this mold section.
  • the upper glass plate 38 is placed on top of this assembly with tubular connector 20 extending through the aforementioned hole 40 in the plate 38 Prior to assembly of the upper glass plate 38, the upper mold section 28 is fitted in the aforementioned manner on the lower mold section 26. The assembly of the upper glass plate 38 is through the upper extremity of the vertical opening through the mold section 28.
  • the floating top 30 of the mold is assembled to the upper mold section 28 with the tubular connector 20 extending through the hole 31 in the top.
  • a suitable weight is then placed on the top 30 to exert a light compressive force on the assembly within the mold.
  • the weighted mold is then placed in a hightemperature furnace is an atmosphere of an inert gas to avoid oxidation and heated at approximately ],700 F for approximately 10 minutes, depending on the masses of the molds in the furnace and the furnace capacity.
  • the mold is heated at this temperature only sufficiently long for the glass materia of the plates 36, 38 under compression as aforesaid, to flow sufficiently to encapsulate the aforementioned assembly in the mold.
  • the glass material conforms to the wall structure of the mold and gases escape around the mold top 30.
  • the glass material conforms closely to the tubing sections, the exposed portions of the tubular connectors and any exposed portions of the aforementioned extension members within the mold, such as the members 48 and 50 for example.
  • the glass material may be annealed by being cooled to 400 F in a cool zone of the furnace, after which the mold is removed from the furnace. After cooling of the parts to handling temperature, the assembly is removed from the mold.
  • the extension members or alignment pins which protrude from the assembly may be removed by a pulling force from the respective tubular connectors 16, 18, 20 and 22. Thereafter an etchant, such as ferric chloride for example, may be pumped through the fluid passages in the assembly to remove the sacrificial tubing.
  • the etchant may be inletted, say through the tubular connector 16, while the tubular connectors 20 and 22 are plugged temporarily, so that the etchant exits through the tubular connector 18.
  • the etchant may be inletted in a similar manner, while the tubular connectors 18 and 22 are plugged, so as to exit from the tubular connector 20.
  • the etchant may be inletted as aforesaid, while the tubular connectors 18 and 20 are temporarily plugged, so that the etchant exits from the tubular connector 22. This removes all of the sacrificial tubingleaving the construction of FIG. 1.
  • the article may'then be cleaned with water and such water may be pumped through the various passageways and tubular connectors associated therewith.
  • the finished product having protruding tubular connectors, is very durable and not prone to breakage.
  • the tubular connectors are so embedded in the glass mass that they very strongly resist breaking off. It is believed made clear that the internal passageways connected to the tubular connectors are formed entirely of exposed glass which is strongly resistant to corrosive attack. It will be obvious from the foregoing that intricate passageways may be formed in a block of slab of glass of monolithic form according to this method of fabrication, which intricate passageways may extend vertically as well as horizontally in the glass mass.
  • extension members ensure that during the encapsulation process the glass material does not flow between the tubular connectors and the corresponding sections of sacrificial tubing, nor between the sections 42, 46 of sacrificial tubing.
  • the bores in the finished article are smooth and need not have restrictions therein such as would interfere with constant fluid flow rates through the bores. It will be evident that in the assembly of the tubular connectors with the sections of sacrificial tubing, the tubular connectors, instead of being socketed in the sacrificial tubing, may provide sockets to receive the sacrificial tubing.
  • one of said tubing sections on preforming has an opening structured in the wall thereof intermediate the ends of the tubing section, and on assembling said tubing sections has the last-mentioned opening socketing an end of another tubing section at the location of said passageway junction.
  • tubing sections are formed of metal
  • preforming of one of said tubing sections includes bending of the last-mentioned section in accordance with said predetermined layout of said passageway.
  • a nipple' formed of erosion-resistant material is positioned and supported adjoining and in communication with one end of one of said tubing sections in the assembly of said tubing sections, said nipple extending without said glass material in the molding step and remaining captive in the glass material after said removal of said tubing sections.

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  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Optical Measuring Cells (AREA)
  • Glass Compositions (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Devices For Use In Laboratory Experiments (AREA)
  • Joining Of Glass To Other Materials (AREA)
US00246966A 1972-04-24 1972-04-24 Method of fabricating laboratory glassware Expired - Lifetime US3770405A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US24696672A 1972-04-24 1972-04-24

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US3770405A true US3770405A (en) 1973-11-06

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US (1) US3770405A (xx)
JP (1) JPS572657B2 (xx)
AU (1) AU470204B2 (xx)
BE (1) BE797164A (xx)
CA (1) CA975560A (xx)
CH (1) CH561669A5 (xx)
DE (1) DE2319974C2 (xx)
FR (1) FR2181920B1 (xx)
GB (1) GB1391400A (xx)
IT (1) IT977868B (xx)
NL (1) NL7302035A (xx)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4015965A (en) * 1975-12-22 1977-04-05 American Optical Corporation Method of making artificial intraocular lenses with holes
US4023597A (en) * 1973-12-20 1977-05-17 Tioxide Group Limited Distributors
US4288238A (en) * 1979-01-08 1981-09-08 Klepsch Kunst Gmbh & Co. Kg Galerie Process and mould for the manufacture of multi-walled hollow bodies, especially of glass
US4326872A (en) * 1980-06-30 1982-04-27 Technology Glass Corporation Method for making perforations or depressions in a glass work piece
US6855251B2 (en) 1998-09-17 2005-02-15 Advion Biosciences, Inc. Microfabricated electrospray device
WO2010126992A1 (en) * 2009-04-28 2010-11-04 Corning Incorporated Microreactors with connectors sealed thereon; their manufacturing

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6289779U (xx) * 1985-11-26 1987-06-09
GB2241233A (en) * 1990-02-21 1991-08-28 Martin Harnett Method of producing perforated glass
DE102019205263A1 (de) * 2019-04-11 2020-04-16 Carl Zeiss Smt Gmbh Verfahren zum Herstellen eines Glaskörpers mit Durchgangskanälen

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2156156A (en) * 1935-07-15 1939-04-25 Mahlck Gustave Method of producing grooves or channels in dielectric materials

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR328563A (fr) * 1903-01-17 1903-07-16 Harry Hogge Procédé pour pratiquer des orifices ou cavités dans le verre
US2072194A (en) * 1934-10-31 1937-03-02 Kimble Glass Co Method of forming canals in glassware
GB846746A (en) * 1957-05-15 1960-08-31 Atomic Energy Authority Uk Improvements in or relating to apparatus comprising glassware

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2156156A (en) * 1935-07-15 1939-04-25 Mahlck Gustave Method of producing grooves or channels in dielectric materials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
A.P.C. Application Serial No. 125,892, B. Wempe, April 27, 1943, 2 pgs. spec, 1 sht. dwg. *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4023597A (en) * 1973-12-20 1977-05-17 Tioxide Group Limited Distributors
US4015965A (en) * 1975-12-22 1977-04-05 American Optical Corporation Method of making artificial intraocular lenses with holes
US4288238A (en) * 1979-01-08 1981-09-08 Klepsch Kunst Gmbh & Co. Kg Galerie Process and mould for the manufacture of multi-walled hollow bodies, especially of glass
US4326872A (en) * 1980-06-30 1982-04-27 Technology Glass Corporation Method for making perforations or depressions in a glass work piece
US6855251B2 (en) 1998-09-17 2005-02-15 Advion Biosciences, Inc. Microfabricated electrospray device
US6858842B2 (en) 1998-09-17 2005-02-22 Advion Biosciences, Inc. Electrospray nozzle and monolithic substrate
WO2010126992A1 (en) * 2009-04-28 2010-11-04 Corning Incorporated Microreactors with connectors sealed thereon; their manufacturing

Also Published As

Publication number Publication date
DE2319974B1 (de) 1974-03-21
NL7302035A (xx) 1973-10-26
DE2319974C2 (de) 1974-10-17
GB1391400A (en) 1975-04-23
AU5261773A (en) 1974-08-29
DE2319974A1 (de) 1973-11-08
CA975560A (en) 1975-10-07
FR2181920B1 (xx) 1977-09-02
IT977868B (it) 1974-09-20
CH561669A5 (xx) 1975-05-15
AU470204B2 (en) 1976-03-04
FR2181920A1 (xx) 1973-12-07
JPS572657B2 (xx) 1982-01-18
BE797164A (fr) 1973-09-24
JPS4941410A (xx) 1974-04-18

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Effective date: 19871231