US3073357A - Penetrometer and filling device therefor for porosimeters - Google Patents

Description

Jan. 15, 1963 w. c. HAMPTON 3,073,357

PENETROMETER AND FILLING DEVICE- THEREFOR FOR POROSIMETERS Flled May 12, 1958 2 Sheets-Sheet 1 To Ilia/0M Pu MP MERtl/RY Barns INVENTOR. WILL/AM C. HAMPTON WZM' Arm #2 NE Y Jan. 15, 1963 w. c. HAMPTON 3,073,357 PENETROMETER AND FILLING DEVICE THEREFOR FOR POROSIMETERS 2 Sheets-Sheet 2 Filed May 12, 1958 FI'E.4-

Penn/z: I/awn.

. PEN: rkau: ran

8; a rose VAL v:

a Z L 3 w 1 mm 1 v 3 M C I 7 W J M p w a M g H m c Wu M s F U V r w .m 4 1V T V JP n M. O. u or M 5 5 V 4 W m 4 a J!- z 2 5 FILL/M6 D5 VICE Pecan-0e: Gena-xerox.

INVENTQR. MILL/AM C HA MbroN /Wfi? F'Il3.5

Arrolz NE Y test. Tlivoluuie ofpenetrati n This invention relates to porosimeters, and more particularly to a penetrometer and a fillnig device there for for use with a porosimeter of the-type employing the mercury intrusion method.

I United States Patent A main object of the invention is to provide a novel 7 and improved penetrometer and a filling device therefor for use in a porosimeter of the type employing the mercury intrusion method to measure the sizes and volumes of the pores of porous materials.

A further object of the invention is to provide an improved penetrometer for use in a porosimeter, said penetrometer being simple in construction, being easy to fill, and which is especially suitable for use in testing powdered samples of material, the penetrometer being formed and arranged so that it is not necesasry to employ means to plug up its capillary stem to prevent the powdered material from entering the capillary passage thereof and 1 so that the inconvenience and inaccuracy involved in using such means is avoided.

A still further object of the invention is to provide an improved penetrometer and filling device therefonfor use in a porosimeter of the type disclosed in US. Patent No;

1 2,886,964 to Justin I. Shapiro and'Nathaniel M. Winslow;

A still further object of the invention is to provide an improvedfillingldevice' for a penetrometer for use in a porosimeter' of the typ'e employing the mercury intrusion method, such as is disclosedin US. Patent No. 2,886,964,

said filling devicebeing arranged so that itis possible to always read the low valued" end of the penetrometer scale while the penetrometer is-installed in its invertedf position in the filling device, and being further arranged so that the pressuresin the lower portions of the-filling 5 7 device are, constantly equalized, whereby 'accurate porosity data at the large pore end'of the porosity spectrum of a sample under test maybe obtained.

Further objects and advantages of the invention willbecome apparent ,from the,;following description and 7 claims, and from the aceompanying' drawings, whereinf FIGURE l is a side elevatiohal view,}partly"in vertical cross-section, of, an improved penetrometer and-"a filling device therefore, constructed in accordance withthe pres-- 'ent invention, the' penetrometer being shown in its inverted position andarranged for filling. y i g Y FIGURE ,2 is a horizontal "cross-sectional view taken on line 2+2 of.FIGURE 1. 4 I

FIGURE 3 is an enlarged vertical cross-sectional view taken through the bulbend of the p'enetrometer. Oil-11 in 3i.of.FIGURE,1.

- -Q+IFIGURE 4i'isia horizontal cross-sectional view-taken 2 bit theline4- 4of FIGURE 3.

, FIGURE 5. isfa;schematic view showinglthe' conduit connections of ressureiin said prespre vessel and containing th' shown in FIGURE 1.

Patented Jan. 15, 1963 ice cation of pressure, at each pressure, is read on the cali-' brated stem of the penetrometer, which is visible through a transparent Window section of the pressure vessel.

The porosimeter includes respective pressure gauges 21,

"32 through a cross fitting 36. A hydraulic fluid supply conduit 34, provided with a manually controlled valve 28 is connected between a fluid reservoir and the pressure generator 24. Gauge 23 is connected through a conventional gauge protector 38 and a conduit 39 to cross fitting 36. 7

Gauge 22 is connected through a conventional gauge protector 40 and a conduit 41, including a manually controlled cutofi valve 42, to the cross fitting '36.

Gauge 21 is connectedthrough a conduit 44- and a vacuum cut-off valve 45'to a conventional external vacuum pump. Also connected to the conduit 44 is a conduit 47 connected to the upper conduit-connection tube 48 of a filling device 49, shown in detail in FIGURES 1 and 2.

Filling device 49 comprises an upper chamber element 50 and'a tubular lower chamber element 51 having a tapered. top end portion 52 adapted to be sealingly and detachably secured in the downwardly flaring lower end portion 53 of upper chamber element 50. Chamber eletion 55 adapted'to supportingly receivethe end of the calibrated tube portion .56 ofjthe penetrometer 57, as

Integrally formed with thebottom of the conical member'55 anddepending axially therefrom is a conduit 55" provided with a manually operated cut-oflf valve 56,

leading to a spherical reservoir 57; integrally connected to the end of the conduit 55'. A pressure-equalizingconduit 58v connects reservoir 57' to a portion of tubular Chamber 51 is provided with a horizontally extending conduit element 59 provided with a three-way stop cock.

'64}, formed with an atmospheric vent conduit 61 andanother conduit 62,. said stop cock being of conventional 4 construction. The'stopcock6ilis providedwith an' "operating' element 63"which maybe rotated to respective diiferent positionsin which the stop cock (1).seals'otf i conduit59, (2) connects conduit '59to conduit 62, or.(3)

- connectsconduit 591 to atmospheric vent conduit 61.

As shown in FIGURE 1, the downwardly flaring skirt member 5.3.is formed at its lower end with a peripheral f bead 6:3. Abovesaid head, the skirt member-531s pro vided with respectiveupwardly-and ontwardly' projecting l 1 ugs. 61f; 6-1'. 'The upper portion of chamber 51-is5pro f videdwith respective downwardly and outwardly extenda lugs 56 62 lq atedb w t emes 6 611 R Pec tivelcoiled fastening springsfiia' are. detachably fastened eir endst pairs of'lugs 61', 62". and engage o the spring 'acts to{ retain the. skirt member "53injsealin' I lin up l. v

s rneter, as described in a e e the veri n f h s we, h'w e l .as shownin FIGURE :1, whereby theztension lso'ta djustably: supported aining?suitable hydraulic, Ike, theco'nduit being supply valve 28. Also supported on this bracket is another bottle adapted to contain mercury, said last-named bottle being located below the filling device 49 and being so arranged that the depending vertical portion 72 of the conduit element 62may be at times engaged through the neck of the bottle into the mercury contained therein, whereby mercury may be admitted into conduit 59 and into the filling device, as will be presently described.

The chamber elements 59 and 51 are formed of suitable transparent material, such as glass, or the like.

The penetrometer 57 comprises the calibrated glass stem 56, open at one end 73 and formed at its other end with a flaring bell-shaped member 74 having an outwardly projecting to'p flange 63' provided with a ground flat annular top surface 64'. A ground flat disc 65' is engaged on the top surface 64', the contacting surfaces being preferably coated with a light film of sealing material, such asv silicon grease. A cylindrical metal ring member 66 surrounds fiange 63' and disc 65" and is formed with an inturned bottom flange 67 which underlies flange 63'. The upper portion of ring member 66' is formed with internal threads 68 with which are threadably engaged the external threads 69 of an annular clamping ring 7t). An O-ring 71 of resilient deformable material, such as rubber, or the like, is engaged between the bottom end of ring 70 and the peripheral margin otdisc 65. Ring 70' is provided with a serrated top flange 79' which is substantially equal in outside diameter to the ring member es, whose outside surface is similarly serrated.

The penetrometer stem is extended upwardly inside member 74, as shown at '72, so that it terminates a very short distance below the cover disc 65', and is bevelled at its top end, as shown at 73. Thus, there isidefined an annular space 74' around the extension 72, adapted to receive the-material under test, for example, powdered material 75. The open end of extension 72' is above the surface of the sample 75' when the penetrometer is held in its customary upright position during loading of the test sample in annular space 74, thus preventing the sample from sliding down the capillarybore 76. When the mercury rises in this annular space 74 it floats the sample up to the top of the space; but since the mercury is flowing into the space via the open end of extension 72', the sample cannot escape down the bore.

As is fully described in U.S. Patent No. 2,886,964, the

bottom member 31 of'pressure vessel 32 is formed with an internal cavity adapted to receivethe sample-containing bulb portion of the penetrometer when the penetrometer is in its working position (inverted as compared with the position thereof shown in FIGURE 1), and the pressure vessel 32 is provided with a neck portion 81 having an internal bore of sufiicient size to freely receive and ver tically support the penetrometer stem 56 therein. The calibated stem of the penetrometer is visible through a vertical transparent window provided inthe observation chamber 86.

In determining the pore sizes and volumes of a material, a weighed sample 75, of known volume or density,-ofi

the material is placed in thepenetromcter sample space 74 and said space is sealed by fastening the cover disc' 65' I'COILZIHd securing same on the sealing surface 64- by means of the elements 66', 7d and 717,-as shown in FIGURE 3. The penetrometer 57 is-then placed, stem down, in the filling device 49, Which is' then-closed, as shcwnin FIGURE '1, and is corinectedno thevacuurn pump by the conduit 7 engaged on the' tub e element; d8, .as'abovedescribed. i

p it The mercury bottle is .thenclamped position with the. mercury filling tube '1; well below-the su'rtacc. of

With vacuum valve t open andjthe device j the mercury,

draw mercury just beyond the stop cock into conduit 59, but not into the filling chamber.

The filling chamber is then evacuated to a pressure below 100 microns, after which vacuum valve is closed.

Suflicient mercury to fill the penetrometer 57 is then admitted into the filling device by means of stop cock 60. At this time the valve 56' is closed, so that the mercury accumulates around the bottom end of stem 56 in conical portion 55. i

The stop cock 6% is then carefully manipulated to admit air into the filling device, forcing the mercury into the penetronieter, the stop cock 66 being closed at an air pressure in the filling chambersufiicient to completely fill the penetrometer, the value of said pressure being indicated on gauge 21.

Following this, valve 56 may be opened to allow the excess mercury to drain into bulb 57, whereby the calibrations on the end of stem 56 may be observcd for subsequent changes in the air pressure in the filling chamber, with the apparatus in the position of FIGURE 1.

Thus, stop cock 6:) may be further manipulated to allow the air pressure in the filling chamber to increase, whereby the mercuryy in the penetrometer bore will be forced upwardly in accordance with the penetration of the mercury into the sample 75 as the air pressure increases.

The above procedure allows the porosity data for the sample material to be obtained at the large pore end of the spectrum, namely, the data derived from the displacement of the end of the mercury column relative to the calibrations on stem 56 as air is admitted to increase the pressure in the filling device in steps up to and including atmospheric pressure. r

After this preliminary data has been obtained, the filling device 49 is carefully nnfastened fromits clamps and inverted, Ibeing refastened to its clamps in inverted position. The drop in level of the mercury columnin stem 56, corresponding to the volume of pores entered at this pressure, is then noted, said pressure being the sum of the pressure due to the height of mercury above; the sample (1 inch of mercury=0.492 pound per square inch gauge) and the indicated absolutepres'sure (atmospheric pressure). p i

The penetrometer 57 is then carefully removed from the filling device 49 and is placed in the pressure vessel 32 for the continuationof the test, as described in U.S.

Patent bio-2,886,964. Thus, the penetrometer is in serted in the pressure vessel with its bulb portion housed in the member 31 and the calibrations on the stem 56 facing outwardly and visible through the transparent Window of observation section 86. The hydraulic fluid bottle 7 (connected to conduit 34 through valve 28) is then raised to an elevated position such that liquid emerges from the bleeder valve 90, and is secured in said position, the

' jbleederwalve 90 being then closed. Valve 28 is'then closed; and the pressure in chamber 32 is then raised by rotating the handle 27 of the pressure generator 24, the pore volumes and pore diameters (as related to gauge pressures) being noted from the mercury column in stem 56, at appropriate intervals. Since stem Si t-is open at 'its top end, the pressure'in chainbert32 is applied" to the mercury column in" said stern andgtof the mercury in space 74', causing the height of said mercury column to change withthe variations in pressure.- i i cock" its closed :to ace ates er and conduit 62;- the vac uum pu'mp is started. ilhestock' cock is then'care-v fullyfimanipulated by means of its value ;handlef63 to.

' {When a. pressure of about 250p'ounds per square inch is. reached, valve 42 is'closed, the-higher=pressures being U- When the pore size spectrurn'readingis have been pb- ,taincdiover.theLdesired pressurej range,=fthej presiiur'e :is relieved 'byrbacking ofl.the pressure. generator ioperatirig screw slightly Valve. '28, hl'eeder valve sc am valve 42 are then opened..-; 1The.hydraulicfluid"-@supply bottle is then lowered toga' position below the top rim of them is her 31, allowingtthe instrument,to. drain."-- The pressure vessel fiz is their opened and the penetrorrieter} 57 it;

sprees? removed, whereby the apparatus isreadyfor another determination.

While a specific embodiment of an improved apparatus for measuring the pore sizes and volumes of pores in material has been disclosed in the foregoing description, it will be understood that various modifications within the spirit of the invention may occur to those skilled in the art. Therefore it is intended that no limitations be placed on the invention except as defined by the scope of the appended claims.

What is claimed is:

1. In a porosirneter, a penetrometer filling device comprising an elongated chamber adapted to receive a penetrometer in an upright position therein, a first conduit element communicatively connected to said chamber and adapted to be connected to a vacuum pump, a second conduit element communicatively connected to said chamher and adapted to be immersed in a quantity of filling liquid, air vent conduit means, valve means interconnecting said second conduit element, said air vent conduit means and said chamber and being formed and arranged to selectively control communication between said air vent conduit means and said chamber and between said econd conduit element and said chamber, a convergent end wall portion in said chamber supportingly engage able with the open end of a penetrometer disposed in upright position in the chamber, a reservoir bulb subjacent said convergent end Wall portion, conduit means communicatively connecting said bulb to the bottom of said end wall portion, and a cut-off valve in said lastnamed conduit means.

2. In a porosimeter, a penetrometer filling device comprising an elongated chamber adapted to receive a penetrometer in an upright position therein, a first conduit element communicatively connected to said chamber and adapted to be connected to a vacuum pump, a second conduit element communicatively connected to said chamber and adapted to be immersed in a quantity of filling liquid, air vent conduit means, valve means interconnecting said second conduit element, said air vent conduit means and said chamber and being formed and arranged to selectively control communication between said air vent conduit means and said chamber and between said second conduit element and said chamber, a convergent end wall portion in said chamber engageable with the open end of a penetrometer disposed in upright position in the chamber, a reservoir bulb subjacent said convergent end wall portion, conduit means communicatively connecting said bulb to the bottom of said end wall portion, a cutofl valve in said last-named conduit means, and further conduit means communicatively connecting said bulb to a point in said chamber spaced a substantial distance above said convergent end wall portion.

3. In a porosimeter, a penetrometer filling device comprising an elongated chamber adapted to receive a penetrometer in an upright position therein, a first conduit element communicatively connected to the upper portion of said chamber and adapted to be connected to a vacuum pump, a second conduit element communicatively connected to the intermediate portion of said chamber and adapted to be immersed in a quantity of filling liquid, air vent conduit means, valve means interconnecting said second conduit element, said air vent conduit means and said chamber and being formed and arranged to selectively control communication between said air vent conduit means and said chamber and between said second conduit element and said chamber, a restriction in said chamber adjacent the bottom end thereof and below the connection of said second conduit element to the chamber, defining a reservoir bulb at said bottom end ti and defining a convergent wall portion above said reservoir bulb adapted to supportingly engage the open end of a penetrometer disposed in said chamber, and a manually controlled valve mounted in said restriction.

4. In a porosimeter, a penetrometer filling device comprising an elongated chamber adapted to receive a penetrometer in an upright position therein, a first conduit element communicatively connected to the upper portion of said chamber and adapted to be connected to a vacuum pump, a second conduit element communicatively connected to the intermediate portion of said chamber and adapted to be immersed in a quantity of filling liquid, air vent conduit means, valve means interconnecting said second conduit element, said air vent conduit means and said chamber and being formed and arranged to selectively control communication between said air vent conduit means and said chamber and between said second conduit element and said chamber, a restriction in said chamber adjacent the bottom end thereof and below the connection of said second conduit element to the chamber, defining a reservoir bulb at said bottom end and defining a convergent wall portion above said reservoir bulb adapted to supportingly engage the open end of a penetrometer disposed in said chamber, a manually controlled valve mounted in said restriction, and conduit means communicatively connecting said reservoir bulb to a point in said chamber spaced a substantial distance above said restriction.

5. The structure of claim 4, and wherein said point is located between said secondconduit element and said restriction.

6. In a porosimeter, a penetrometer filling device comprising an elongated chamber adapted to receive a penetrometer in an upright position therein, a first conduit element communicatively connected to the top end portion of said chamber and adapted to be connected to a vacuum pump, a second conduit element communicativly connected to the intermediate portion of said chamber and having an end portion extending substantially parallel to said chamber and adapted to be immersed in a quantity of filling liquid, air vent conduit means, valve means interconnecting said second conduit element,

said air vent conduit means and said chamber and being formed and arranged to selectively control communication between said air vent conduit means and said chamber and between said second conduit element and said chamber, a restriction in said chamber adjacent the bottom end portion thereof defining a reservoir bulb at the lower side of said restriction and defining a convergent wall portion above said reservoir bulb adapted to supportingly engage the open end of a penetrometer disposed in said chamber, a manually controlled valve mounted in said restriction, and conduit means communicatively connecting said reservoir bulb to a point in said chamber spaced a substantial distance above said restriction.

References Cited in the file of this patent UNITED STATES PATENTS 791,480 Maynard June 6, 1905 2,158,102 Betzold et al. May 16, 1939 2,369,591 Marden et al. Feb. 13, 1945 2,495,905 Pogue Jan. 31, 1950 v 2,527,849 Ranney Oct. 31, 1950 2,641,924 Reichertz June 16, 1953 2,676,485 Morgan Apr. 27, 1954 2,696,937 Johnson et a1. Dec. 14, 1954 2,862,307 Bloomer et al. Dec. 2, 1958 2,886,964 Shapiro et a1. May 19, 1959

Claims (1)

1. IN A POROSIMETER, A PENETROMETER FILLING DEVICE COMPRISING AN ELONGATED CHAMBER ADAPTED TO RECEIVE A PENETROMETER IN AN UPRIGHT POSITION THEREIN, A FIRST CONDUIT ELEMENT COMMUNICATIVELY CONNECTED TO SAID CHAMBER AND ADAPTED TO BE CONNECTED TO A VACUUM PUMP, A SECOND CONDUIT ELEMENT COMMUNICATIVELY CONNECTED TO SAID CHAMBER AND ADAPTED TO BE IMMERSED IN A QUANTITY OF FILLING LIQUID, AIR VENT CONDUIT MEANS, VALVE MEANS INTERCONNECTING SAID SECOND CONDUIT ELEMENT, SAID AIR VENT CONDUIT MEANS AND SAID CHAMBER AND BEING FORMED AND ARRANGED TO SELECTIVELY CONTROL COMMUNICATION BETWEEN SAID AIR VENT CONDUIT MEANS AND SAID CHAMBER AND BETWEEN SAID SECOND CONDUIT ELEMENT AND SAID CHAMBER, A CONVERGENT END WALL PORTION IN SAID CHAMBER SUPPORTINGLY ENGAGEABLE WITH THE OPEN END OF A PENETROMETER DISPOSED IN UPRIGHT POSITION IN THE CHAMBER, A RESERVOIR BULB SUBJACENT SAID CONVERGENT END WALL PORTION, CONDUIT MEANS

Images