`Lawhead
`
`3,958,572
`['11]
`[451 May25, 1976
`
`[541 BLOOD COLLECTING AND SEPARATING
`ASSEMBLY STOPPER
`'
`[75] Inventor: Creighton M. Lawhead, Corning,
`
`[73] Assignee: Corning Glass Works, Corning,
`NY.
`
`Dec. 16, 1974
`[22] Filed:
`[21] Appl. No.: 532,828
`
`[52] US. Cl ............................... .. 128/272; 215/247;
`215/320
`[51] Int. Cl.2 ........................................... .. A61J 1/00
`[58] Field of Search .......... .. 128/213, 214 B, 214 D,
`128/2 F, 2 G, 215-217, 218 R, 218 M, 218
`D, 218 DA, 220, 272, 275-276, 297;
`215/247, 355, 296, DIG. 3, 320
`
`[5 6]
`
`References Cited
`UNITED STATES PATENTS
`
`2,607,347
`2,812,231
`
`8/1952 Kleiner ............................. .. 128/276
`11/1957 Zar ........................... .. 128/272 X
`
`2,848,130
`
`8/1958 Jesnig . . . . . . . . . . . .
`
`. . . . . . . . .. 215/247 X
`
`3,136,440
`
`6/1964 Krug et al. ........................ .. 215/247
`
`3,141,460
`3,330,281
`
`7/1964 Tsochatzopoulos .............. .. 128/276
`7/1967 Visser ........................ .. 128/272
`
`3,343,699
`
`9/1967 Nicko . . . . . . . . , .
`
`. . . .. 215/247
`
`3,869,059
`3/1975
`Ellis .................................. .. 215/320
`FOREIGN PATENTS OR APPLICATIONS
`724,915
`1955
`United Kingdom ............... .. 128/272
`407,559
`1934 United Kingdom ............... .. 128/220
`
`Primary Examiner~John D. Yasko
`Attorney, Agent, or Firm—Thomas J. McNaughton;
`Burton R. Turner; Clarence R. Patty, Jr.
`
`ABSTRACT
`[5 7]
`A stopper for use with an evacuated blood collecting
`and separating tube comprising a ?ange portion, a
`plug portion depending from the ?ange portion in
`cluding a generally frustoconical lateral face and a ?at
`annular bottom face, and a nose portion depending
`from an inner circumference of the plug bottom face.
`The nose portion includes a beveled or tapered sec
`tion having an axial cavity extending through the nose
`portion into the plug portion. The axial cavity prefer
`ably includes a frustoconically shaped lateral face.
`2 Claims, 4 Drawing Figures
`
`Bass and Spangenberg
`v.
`Fresenius Kabi USA, LLC
`U.S. Patent No. 8,476,010
`Exhibit 1034
`
`
`
`US. Patsnt May 25, 1976
`
`3,958,572
`
`8 3
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`\\\\\\\\\\\\\\\
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`I15, __\
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`1
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`3,958,572
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`BLOOD COLLECTING AND SEPARATING
`ASSEMBLY STOPPER
`
`BACKGROUND OF THE INVENTION
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`1. Field of the Invention
`This invention relates to blood collecting and sepa
`rating tube assemblies and more particularly to punc
`turable stoppers used to form a vacuum-tight and liq
`uid-tight seal within the open end of a blood collecting
`and separating tube.
`2. Prior Art
`Evacuated tubes have been used to collect and sepa
`rate blood for some 20 years. The conventional tube
`assemblies include a cylindrical container or tube hav
`ing a closed end and an open end vacuum sealed by
`means of a removable needle-pierceable stopper or
`closure. Typically blood is withdrawn from a patient by‘
`?rst puncturing a vein with one end of the double
`ended needle and then while ?rmly securing the hous
`ing holding the needle, pushing the needle pierceable
`closure of a collection tube against the other end of the
`needle until the closure is pierced. The partial vacuum
`within the collection tube results in siphoning or with
`drawing blood into the tube. After the desired volume
`of blood is drawn into the tube, the needle is withdrawn
`from the patient. An example of a conventional blood
`collecting and separating tube is described in U.S. Pat.
`No. 2,460,641.
`The standard venipuncture procedure is usually ac
`complished with the stoppered end of the container
`being held downwardly. Accordingly, as blood is si
`phoned into the tube, the blood will rest against the
`inner surface of the stopper, that is, at the bottom end
`of the stopper. After venipuncture, it has been found
`that with known container assemblies a small portion of
`the blood remains attached to the bottom end of the
`stopper and also between the stopper and container
`walls.
`The major failing of the standard stopper, from the
`user standpoint, is its retention of a substantial portion
`of clotted blood or cells at the stopper-container wall
`juncture even upon completion of the centrifugation of
`the blood. This failing makes it highly desirable, if not
`essential, to remove the stopper before centrifugation
`and clean (using a swab or stick) the clot or cells from
`the top inside wall of the tube.
`Merely removing the stopper without cleaning the
`residual ring-clot or cells will not overcome the prob
`lem, since centrifugal force does not remove the un
`wanted attachment of clot or cells from the tube wall
`because of the drying onthe wall that begins to occur
`just after the stopper is removed or “popped”. This
`drying and adhering of clot or cells on the tube wall has
`been found to be aggravated during centrifugation both
`by turbulent air action and by rising temperatures
`within the centrifuge, throughout the duration of the
`spin, which is typically, eight to twelve minutes. .Clean
`liness of the tube wall after centrifugation is highly
`60
`desirable because most serum is poured from the tube,
`and attached cells can thus be eluted by the pouring of
`the serum or plasma.
`Under present practices requiring the removal of the
`stopper prior to centrifugation, a period of up to three
`hours may elapse between centrifugation and serum or
`plasma utilization, during which time the blood sample
`is open to the atmosphere and evaporation of gaseous
`blood constituents may take place. The net result may
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`be an increase in the apparent concentration of some
`blood constituents and a decrease in the apparent con
`centration of the gaseous constituents, which produces
`a deviation from the true clinical values of serum or
`.plasma chemistries for the patient in question.
`Also while the unstoppe‘red tube is standing in a rack
`waiting to be analyzed, particulate matter and other
`airborne contaminants, as well as splashed reagents or
`splashed serum from other tubes (occurring when
`tubes are hastily put into a common rack), can readily
`contaminate the blood sample prior to analysis.
`The over-riding concern with blood collecting and
`separating tube assemblies which require stopper re
`moval is, however, the potential hazard to laboratory
`personnel. The removal of the stopper, the rimming
`with a stick or swab to remove the ring clot, the aerosol
`effect created by the centrifuge rotation, and the possi
`bility of accidental spillage all jeopardize the well-being
`of laboratory workers.
`Also since cells trapped between the stopper and the
`tube walls may be ruptured when the stopper is re
`moved, which results in the exuding of lactic dehydro
`genase (LDI-I), falsely elevated LDl-I levels in the
`serum or plasma analysis may be produced.
`Accordingly, it is an object of this invention to pro
`vide a stopper for use in combination with a blood
`collecting and separating container which will over
`come the disadvantages of prior stoppers.
`Also it is an object of this invention to provide a
`stopper which is easily insertable and removeable from
`a blood collecting and separating tube, and yet which
`maintains an adequate vacuum-tight seal for a pro
`longed storage time.
`It is a further object of this invention to furnish a
`stopper of such a construction that the entire circum
`ferential junction of the stopper and tube inner face is
`maintained in a ?uid tight con?guration to preclude the
`possibility of blood portions from being lodged be
`tween the stopper and tube wall.
`Another object of this invention is to provide a stop
`per having a bottom axial cavity con?guration which
`causes blood adhering within the cavity to flow from
`the cavity during an angle-head mode of centrifugation.
`It is also a major object of this invention to provide a
`stopper suitable for use with a closed-system blood
`collecting and separating assembly having either a gel
`like barrier material initially positioned at the closed
`end of the tube, such as the assembly disclosed in U.S.
`Pat. No. 3,852,144 or a resilient spool barrier means
`initiallly positioned adjacent the stoppered end of the
`tube, as described in U.S. Pat. No. 3,814,248. The
`closed-system assembly may be used to collect blood,
`centrifugally separate blood into at least two phases,
`and automatically partition the separated phases with
`the gel-like barrier material and/or the spool. To assure
`that the separated phase above the barrier, which may
`be serum or plasma, is not contaminated before or
`during pour-off of such phase, it is important that no
`blood constituents remain in the vicinity of the juncture
`of the stopper and tube wall or in an axial cavity in the
`bottom of the stopper upon completion of centrifuga
`tion, and the stopper of the present invention not only
`inhibits the formation of ring clotting but also facili
`tates the removal of such constituents during centrifu
`gation.
`
`
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`3,958,572
`
`20
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`35
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`4
`FIG. 3 is an elevational view partially in section of a
`blood-collecting and separating assembly of the present
`invention.
`FIG. 4 is a fragmental elevational view in section of
`another embodiment of the stopper of the present in
`vention.
`
`3
`SUMMARY OF THE INVENTION
`In accordance with the present invention, the above
`stated objects are achieved by providing, in combina
`tion, a tubular container or tube having a cylindrical
`wall which is closed at one end and open at the other
`end, the open end lying in a plane normal to the axis of
`DESCRIPTION OF THE PREFERRED
`the cylindrical wall; and a stopper symmetrical about a
`EMBODIMENTS
`centerline or axis comprising a ?ange portion, a plug
`A conventional blood collecting and separating con
`portion having a frustoconical outer periphery or lat
`eral face extending downwardly from the ?ange por
`tainer or tube 10 as shown in FIG. 3 is formed of glass
`tion, and a radially recessed nose portion projecting
`or other suitable material to hold a partial vacuum and
`downwardly from the plug portion and having an axial
`to contain blood and includes a cylindrical wall 12
`cavity formed therein. The flange portion has a ?at
`having a smooth inner surface or face 14 which is
`closed at one end 16 and open at the other end 18, with
`bottom annular band or face adjoining an upper cir
`cumference of the plug portion, with the ?ange bottom
`open end 18 lying in a plane normal to axis B—-B of
`wall 12. Vacuum-tight sealing of open end 18 is accom
`band lying in a plane normal to the stopper centerline.
`plished by a stopper 20 formed from a ?exible punctur
`The plug portion has a bottom annular band or face
`able material, such as butyl rubber or other suitable
`lying in a plane normal to the stopper centerline, that
`is, parallel to the ?ange bottom face. The outer circum
`material.
`The stopper, illustrated in FIGS. 1—3 is symmetrical
`ference or edge of the plug bottom band has a diameter
`about a centerline or axis A—A and includes a ?ange
`greater than the inner diameter of the tube wall to form
`portion 30 for overlying open end 18, an integral plug
`a liquid-tight seal with the inner surface of the tube
`portion 50 extending downwardly from flange portion
`wall. When the stopper is fully inserted into the tube,
`30 for forming a vacuum-tight and liquid-tight seal with
`the ?ange portion abuts the open end of the tube, with
`the inner surface 14 of cylindrical wall 12, and an inte
`the entire outer circumference of the plug bottom band
`gral radially recessed nose portion 70, projecting down
`forming a ?uid-tight seal with the tube; and since the
`wardly from plug portion 50 for facilitating the ?ow of
`plug and ?ange bottom bands are parallel, the plane of
`blood portions from the vicinity of the stopper toward
`the plug bottom face is approximately normal to the
`container closed end 16. Flange portion 30 has a lateral
`adjacent inner surface of the tube cylindrical wall.
`face which may be formed by an upper frustoconical
`The nose portion connects with or extends from the
`section 34 and a lower frustoconical section 36; a top
`plug portion at an inner circumference of the plug
`portion bottom hand and thus, upon insertion of the
`or upper face 40 having an axial recess 42 therein; and
`a bottom annular face or band 38 lying in a plane which
`stopper into a tube, the nose portion is spaced apart
`is normal to centerline or axis A—A of stopper 20.
`from the tube inner surface by the width of the plug
`Plug portion 50 includes a radially inwardly and
`bottom band. The nose portion includes a beveled or
`downwardly tapered or frustoconical lateral face 52
`frustoconical outer peripheral face section which pref
`depending from ?ange bottom surface or band 38, and
`erablyjoins the inner circumference of the plug bottom
`a bottom annular face or band 54 lying in a plane nor
`band by means of a short cylindrical section or by a ?rst
`40
`mal to axis A—A and bounded by lateral face 52 along
`inwardly rounded section and a second outwardly
`a lower edge 56 forming an outer circumference of
`rounded portion adjoining a lower circumference‘of
`band 54. Preferably, an annular recess or groove sec
`the ?rst rounded section.
`The nose portion includes a bottom-open axial cavity
`tion 44 connects an inner circumference of the bottom
`face 38 of ?ange portion 50 with an upper edge 58 of
`which may be formed in a bottom surface or in the
`plug lateral face 52. The upper edge 58 of plug lateral
`frustoconical face section of the nose portion. In both
`embodiments, the bottom-open axial cavity preferably
`face 52 has a diameter suf?ciently greater than the
`inner diameter of tube wall 12 to provide for a vacuum
`includes a lateral inwardly and upwardly tapered or
`tight seal between at least an upper portion of conical
`frustoconical face designed to ?ow blood portions from
`surface 52 and the inner surface 14 of tube wall 12. The
`the cavity.
`lower edge 56 of plug portion 50 has a diameter greater
`In order to assure squareness of sealing of the stopper
`than the inner diameter of tube wall 14 to form a liquid
`within the tube, the bottom face of the ?ange and
`tight seal therewith.
`upper edge or circumference of the plug are preferably
`Nose portion 70 connects with and extends from an
`connected with a circumferential recess or groove sec
`inner circumference of plug bottom annular face 54.
`tion. Also, to facilitate insertion and removal of the
`55.
`Nose 70 has an outer face including an inwardly and
`stopper made from a rubber-like material, a lubricant,
`downwardly beveled or tapered frustonical section 74
`such as a silicone oil or aqueous glycerine solution, may
`and an axial bottom-open cavity 82. The cavity 82 is
`be applied to the stopper.
`formed in the underside of the nose portion 70 and
`DESCRIPTION OF THE DRAWINGS
`extends upwardly through nose portion 70 and partially
`through plug portion 50. As shown in FIGS. 1-3, nose
`In order that the invention may be readily carried
`70 includes a ?rst inwardly rounded section 76 adjoin
`into effect, it will now be described in greater detail, by
`ing an inner circumference of plug portion annular
`way of example, with reference to the accompanying
`drawings, in which
`bottom band 54 and a second rounded section 78 con
`necting a lower circumference of ?rst rounded section
`FIG. 1 is a cross-sectional view in elevation of an
`76 with an upper circumference of frustoconical sec
`embodiment of the stopper according to the invention
`tion 74, thus in effect joining the frustoconical secstion
`taken along line I—I of FIG. 2.
`74 to annular bottom band 54 by means of a short
`FIG. 2 is an axial or bottom plan view of the stopper
`cylindrical section with rounded ends.
`as viewed along line II—II of FIG. 1.
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`As illustrated in FIG. 1, nose portion‘70 may have an
`annular bottom face 80 normal to axis A—A into which
`axial cavity 82 is formed. Another embodiment, as
`depicted in FIG. 4, includes a nose portion 70 having
`an axial cavity 82 formed in the frustoconical section
`74 of the nose, thus forming a sharp or acutely angled
`edge 84 at the mouth of the cavity. In both embodi
`ments, cavity 82 is preferably de?ned by an inwardly
`and upwardly tapered or frustoconical lateral face or
`peripheral wall 86 and an upper face‘ 88..T0 assure
`proper needle penetration, upper face 88_is preferably
`flat. Cavity 82 extends through nose portion 70 ,and
`through part of plug portion 50, that is, to a position
`above plug bottom band 54. -
`a
`_
`.
`In the embodiment of stopper 20 illustrated inFIG. 4,
`the nose portion includes a cylindrical section 90 con
`necting the lower circumference of ?rst rounded sec
`tion 76 with frustoconical section 74. Also, the embodi
`ment includes a nose portion having a more steeply
`inclined cavity lateral face 86 and a ,less steeply in
`clined nose portion conical face section 74.
`By way of example, the following dimensions and
`angles are given to more speci?cally describe the stop
`per of the present invention. For a tube 10 having an
`25
`inner diameter of about 0.543 inches, the plug portion
`50 may have a major diameter at upper edge 58 of
`about 0.590 inches, minor diameter at lower edge 56 of
`about 0.550 inches, and a vertical length between
`edges 56 and 58 of about 0.240 inches. Groove section
`44, in the form of a radiused recess, may have a width
`or diameter of about 0.020 to 0.025 inches. Annular
`bottom band 54 of plug portion 50 may have a radial
`width of about 0.030—0.055 inches. An angle included
`upwardly between the intersection of axis A—A with a
`line lying in frustoconical face section 74 of nose por
`tion 70 and lying in a vertical plane intersecting axis
`A—A may range from 40° to 60°. An angle included
`between the intersection of axis A—A with a line lying
`in cavity frustoconical face 86 and in a vertical plane
`intersecting axis A—A ranging from about 15° to 40°
`has been found to be compatible with known angle
`head and flat-out centrifugation.
`If the stopper 20 is made from butyl rubber, the ap
`plication of a slight amount of libricant to the stopper is
`desirable to facilitate insertion and removal of the stop
`per from an evacuated collecting and separating tube.
`Known commercially available silicone ?uids or oils,
`such as manufactured by Dow Corning, or aqueous
`glycerine solutions have been found to be suitable lu
`bricants. The silicone or glycerine treatment not only
`assures enough lubricity for the bottom edge of conical
`plug face to ease into the 90° departure angle with the
`' tube wall after stopper insertion, but also gives added
`protection against cell or clot adherence to the stopper.
`FIG. 3 shows the stopper 20 fully inserted into tube
`10. The assembly is evacuated prior to stopper inser
`tion and blood may be drawn into the assembly accord
`ing to conventional venipuncture practice, such as with
`a double-ended needle device shown in US. Pat. No.
`2,460,641 to Kleiner. The construction of the stopper
`is such that annular groove or recess section 44 permits
`tube open end 18 to abut, without obstruction against
`the ?at bottom face or band 38 of ?ange 30. Due to the
`fact that tube open end 18 lies in a plane normal to the
`tube axis B—B and that plug bottom band 54 lies in a
`plane parallel to flange bottom band 38, plug bottom
`band 54 will also lie in a plane normal to axis B—~B,
`thereby providing an angle of departure of about 90°
`
`3,958,572
`between the plane of plug band 54 and vertical inner
`wall surface 14. That is, when fully assembled, plug
`‘band 54 is normal to wall face 14. Moreover, the unob
`structed abuttment of the ?ange bottom band 38
`against the tube open end 18, accomplished by means
`of,‘ groove section 38, assures squareness of seating and
`precludes cocking or separating of portions of edge 56
`of. bottom band 54from adjacent tube wall portions,
`which would provide an acutely angular space for cells
`or other blood constituents to lodge.
`The 90° angle of departure in conjunction with the
`spacing~apart of .nose portion 70 by the width of plug
`‘bottom band .54 provide ‘for .freedom from ring-clog
`retention at the juncture of the stopper 20 and the tube
`inner wall14. Any blood iadheringto the stopper or
`tube walljn the vicinity of the juncture before centrifu
`gation of the ?lled assembly readily ?ows from the
`annular band ‘54 upon centrifugation of the assembly.
`Also, the. downward and inward slope of frustoconi
`cal section 74_of nose portion 70 and the inward and
`upward slope of frustoconical lateral face 86 of plug
`bottom cavity 82 work in concert to provide a clot-free
`geometry in both angle-head and horizontal modes of
`centrifugation. Blood portions initially adhering within
`cavity 82 and between the outer surface of nose portion
`70 and tube wall 14 readily flow during centrifugation
`down cavity lateral surface 86 and nose portion frus
`tonocical section 74, respectively, and are slung from
`the stopper from near the bottom edge of cavity 82
`toward the bottom of the tube. The frustonocical con
`?guration of cavity lateral face 86 has been found to
`completely eliminate any concern of cellular retention
`on the cavity lateral face 86 resulting from centrifugal
`forces exerted in centrifuges having angle-head rotors.
`Speci?cally, in a typical centrifuge having an angle
`head rotor, the tube 10 is spun about an axis of rotation
`at an angle of about 35° between the axis B—B of the
`tube and the axis of rotation of the rotor. When posi
`tioned within an angle-head rotor, blood within the
`stopper bottom cavity is forced away from the axis of
`rotatin during centrifugation, and toward the outer
`sloped or tapered cavity wall. The slope of the cavity
`lateral face 86 is adapted to enhance ?ow from the
`outer half of the cavity and precludes the possibility of
`blood building up and drying on the cavity wall 86. The
`cleanliness of the stopper cavity is important, because
`subsequent to centrifugation, the stoppered tube (if it
`has a gel-like barrier, as described above) may be
`rested in a horizontal position, thus bringing the sepa
`rated serum into contact with the stopper bottom cav
`ity 82.
`Furthermore the downwardly and inwardly tapered
`or frustoconical shape of plug portion 50 in conjunc
`tion with the construction of the upwardly and inwardly
`tapered bottom cavity 82 extending into a portion of
`plug portion 50 (that is, at a position above bottom
`annular band 54) provides for a stopper which can be
`easily inserted into and removed from the tube open
`end 18, while yet providing excellent vacuum retention
`at or near upper edge 58 and a fluid-tight seal at the
`lower edge 56 of the plug portion 50 of the stopper.
`The invention is not restricted to the examples de
`scribed but also includes various modi?cations and
`constructions for example, a stopper in which the lat
`eral radially downwardly tapered face 52 of the plug
`portion 50 is slightly outwardly curved or bulged, a
`stopper in which the bottom cavity 82 formed axially
`the nose and plug portions 70 and 50 is generally semi
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`spherical in shape, a stopper the nose portion of which
`includes an outer inwardly beveled section 74 having a
`slightly curved cross-section, or a stopper the ?ange 30
`of which includes a cylindrical section overlapping the
`tube open end 18 and extending downwardly over an
`upper end portion the outer surface of tube wall 12.
`I claim:
`1. A stopper assembly for use in combination with a
`tubular blood collection and separation container hav
`ing cylindrical sidewalls de?ning a longitudinal axis and
`provided with an open end portion comprising, a re
`movable stopper including a ?ange portion having
`means for engaging said open end portion of said con
`tainer in a plane substantially normal to the longitudi
`nal axis of the cylindrical sidewalls thereof, a frustocon
`ical plug portion integrally depending from said ?ange
`portion having lateral face means of greater diameter
`than the inner diameter of said sidewalls for sealingly
`engaging said sidewalls in a ?uid and vacuum tight
`relationship, said plug portion tapering inwardly away
`from said ?ange portion and terminating at an annular
`
`3,958,572
`8
`band extending radially inwardly from said lateral face
`means in a plane lying normal to said longitudinal axis,
`a nose portion depending from said plug portion and
`bounded at its juncture with said plug portion by an
`inner circumference of said annular band, said nose
`portion including a lateral face of a frustoconical shape
`which tapers inwardly in a direction projecting away
`from said annular band and an inner face of a generally
`frustoconical shape which tapers inwardly within said
`nose and plug portions in a direction projecting toward
`said ?ange portion, and said annular band providing
`means for spacing said nose portion radially inwardly
`away from the inner surface of said sidewalls to thereby
`facilitate during centrifugation the ?ow of blood com
`ponents away from said sidewalls and across said annu
`lar band toward said frustononical lateral face of said
`nose portion.
`2. The stopper of claim 1 further comprising a cir
`cumferential groove section connecting said plug por
`tion with said ?ange portion.
`*
`* * * *
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`UNITED STATES PATENT @FFECE
`CERTIFICATE CF CQRRECTWFJ
`
`PATENT NO. '.
`DATED
`1
`
`3,958,572
`May 25, 1976
`
`iNVENTOR(S) :
`
`Creighton M. Lawhead
`
`It is certified that error appears in the above-identified patent and that said Letters Patent
`are hereby corrected as shown below:
`
`Column 1, line 52, "onthe" should read -—on the--—; Column
`3, line 33, "hand" should read -—band—-; Column 4, line
`56, "frustonical" should read —-frustoconical——-; Column 4,
`line 66, "secstion" should read -*section——; Column 5,
`line 44, "libricant" should read ——lubricant——-; Column 6,
`line 13, "ring-clog" should read -—ring-clot——; Column 6,
`lines 27 and 28, "frustonocical" should read -=~frustoconioal=--;
`Column 6, line 41, "rotatin" should read ——rotation-=-;
`Column 8, line 16, "frustononical" should read
`——frustoconical——°
`
`[SEAL]
`
`> A ttest.‘
`
`RUTH C. MASON
`Arresting Officer
`
`?igmd and gedled This
`Seventh ?ay Q? September 1976
`
`'
`c. MARSHA
`LL D ANN
`( ommissr'uner uj'l’arems and Trademarks