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IS 13781 (1993): Permeable sintered metal materials -Determination of bupple test pore size [MTD 25: PowderMetallurgical Materials and Products]
IS 13781 : 1993
IS0 4003 : 1977
Indian Standard
PERMEABLE SINTERED METAL MATERIALS - DETERMINATION OF BUBBLE TEST PORE SIZE
UDC 669 - 138’8 : 539’217
@I BIS 1993
BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
July 1993 Group Price 2
Powder Metallurgical Materials and Products Sectional Committee, MTD 25
NATIONAL FOREWORD
This Indian Standard which is iclentical with IS0 4003 : 1977 ‘Permeable sintered metal materials -- Determination of bubble test pore size’, issued by the International Organization for Standardization ( IS0 ), was adopted by the Bureau of Indian Standards on the recommen- dations of the Powder Metallurgical Materials and Products Sectional Committee ( MTD 25 ) and approval of the Metallurgical Engineering Division Council.
The text of IS0 standard has been approved as suitable for publication as Indian Standard with- out deviaticns. Some terminology and conventions are, however, not identical with those used in Indi;ln Standards. Attention is especially drawn to the following:
a) Whcrcver the words ‘International Standard’ appear, should be read as ‘Indian Standard’.
referring to this standard, they
b) Comma ( , ) has been used as a decimal msrker while in Indian Standards the current practice is to use a point ( . ) as the decimal marker.
In this adopted standard, reference appears to IS0 2738. The Indian Standard IS 5642 : 1991 ‘Permeable sintered metal materials - Determinatron of density, oil content and open porosity ( second rwision )‘, which is identical with IS0 2738 : 1987, is to be substituted in its place.
In reporting the results of a test made in accordance with this standard, if the final value, cbserved or calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )‘.
IS 13781’ : 1993
IS0 4003 : 1977
Indian Standard
PERMEA~BLE SINTERED METAL MATERIALS - DETERMINATION OF BUBBLE TEST PORE SIZE
1 SCOPE AND FIELD OF APPLICATION
This International Standard specifies a method, known as
the bubble test method, for the determination of the pore
size of permeable sintered powder metallurgical materials,
i.e. filters, porous bearings, porous electrodes and other
parts with interconnected porosity.
NOTE - The bubble test shall be considered as a quality control test and not as a test for defining filter grades or detemining exact pore size and pore size distribution.
The first bubble of gas will form at the pore having the
greatest throat, the throat being the narrowest section of
this pore.
For calcul’ation purposes, it is assumed that this bubble
forms at the end of a capillary tube of circular cross-section
which is initially filled with the sarne liquid of known
surface tension.
For a circular capillary, the diameter is related to the bubble pressure by the equation :
2 REFERENCE
IS0 2738, Permeable sintered metai materials - Determi- where
nation of density and open porosity. d is the capillary diameter corresponding to the bubble
test pore size, in metres;
3 PRINCIPLE
Impregnation of a test piece with a test liquid. Immersion
of the test piece in the test liquid and introduction of a gas
(usually air) into the test piece at gradually increasing press-
ure. Determination of the pressure at which bubbles are
emitted from the surface of the test piece. Evaluation of
the equivalent bubble test pore size by means of a math-
ematical formula.
‘y is the surface tension of the test liquid, in newtons
per metre;
& is the differential pressure, in pascals, across the
test piece under static conditions, i.e.
AP=P, -PI (2)
p, being the gas pressure, in pascals;
p, being the pressure in the liquid at the level of
bubble formation, in pascals :
PI = 9,81 x’ I_‘, X h (5) 4 DEFINITION
bubble test pore size : The maximum equivalent capillary
diameter in the test piece which is calculated from the
measured minimum pressure required to force the first
bubble of gas through the test piece (under standardized
conditions) impregnated with a liquid.
where pr is the density of the test liquid, in kilograms
per cubic metre;
h is the height of the surface of the test liquid, in
metres, above the highest throat in the test piece.
1
IS 13781 : 1993 IS0 4003 : 1977
Liquid pressure p, 7 r Test piece
L Gas pressure pg L Test liquid
FIGURE - Bubble test ammmbly
NOTES 5 APPARATUS
1 The bub:le test pore size corresponds to the minimum differen- tial pl-essure at which constant bubbling first occurs. For this reason, this pressure is sometimes termed “minimum bubble pressure” or “first bubble point”. The corresponding capillary diameter is some- times termed “maximum pore size” or “maximum pore diameter”, or “largest pore size”. However, the maximum pore size determined with this method may be the result of a single local defect, and therefore not representative of the pore population.
5.1 Dry and filtered gas (generally air) supply, at an
adequate pressure.
2 As the gas pressure increases beyond the minimum bubble press- ure (first bubble point), different aspects of bubbling occur on the test piece. The pressure for a given aspect can lead to the definition of a conventional pore sire. For example, the pressure for which a generalized bubbling occurs is frequently specified (foaming over the whole surface). These particular definitions should be agreed between the iupplier and the user. Moreover, the uniformity of distribution of pores approaching the maximum pore size may be observed by gradually increasing the gas pressure. Cracks and clogged areas are easily discerned by this operation.
5.2 Pressure regulator affording constant and precise
control of the gas pressure, i.e. a gradual increase of the
pressure at a predetermined rate, or a stepwise increke of
pressure and the facility to maintain a constant pressure at
each step.
5.3 Flow-meter, if required
3’ The bubble test does not consfitufe a measurement of the maximum size of particle that the permeable test piece will pass (retentivity of a filter). A filter may be expected to retain all par- ticles larger than the maximum pore size as defined by the bubble test; but, because of irregularity in shape of pores and other phenom- ena related to the filtration process, the same filter will retain particles which are much smaller than the maximum pore size. The determination of the size of the largest non-deforming particle which can pass through the porosity requires timeconsuming methods, for example a glass-bead test. For estimation purposes it is useful to take empirical factors, which are to be multiplied with the bubble test pore size calculated ,from equation (1). The factor is about 0.4 for porous metal made from uniform spherical particles; and about 0.2 for porous metal made from irregular
particles.
5.4 Device to measure the effective gas pressure, measuring
to an accuracy of f 1 % (mechanical pressure gauge, or
water or mercury manometer). This device shall be placed
close to the bubble test cell, in order to facilitate the simul-
taneous observation of the bubble appearance and the
pressure value.
5.5 Assembly for observing the bubble appearance at the
surface of the test piece, according to the shape of the test
piece, and for ensuring that the test piece is completely
saturated with the liquid, and immersed under a constant
depth of the liquid throughout the test. If the test piece is
hollow or of a shape other than flat, it should be rotated
with its major axis horizontal so that the whole surface is
examined.
2
IS13781:1993 ISO4003: 1977
5.6 Test liquid, selected in relation to the kind of metal
composing the test piece. Among pure liquids which wet
metals perfectly, 95 % ethanol, methanol, isopropanol or
carbon tetrachloride are most generally employed (see the
table for properties). The test is carried out at room tem-
perature (20 + 5 “C). The surface tension, y, of the test
liquid may be obtained from tables of physical constants.
TABLE - Tast liquids suitable for usa with~parmaable metals
Surface tension Test liquid Density at 20°C
g/cm3 N/m
Methanol 0.79 0,022 5
Ethanol, 95 % 0,805 0,023
lsopropanol 0.79 0,021 5
Carbon tetrachloridel ) 1.59 0.027
1)’ As carbon tetrachloride vapour can be dangerous to health, thk usual laboratory precautions should be taken.
6 PROCEDURE
The test piece shall be clean, dry and free from extraneous
material and any trace of grease or simiiar substances likely
to hinder the perfect and uniform wetting action of the test
liquid.
Impregnate the test piece completely with the test liquid.
insert it in the bubble test apparatus and maintain it fixed,
immersed under the smallest depth of test liquid consistent
with the convenient observation of the appearance of the
bubbles. Measure this depth h (see the figure) and the
temperature of the liquid.
From an effective gas pressure of zero, increase the pressure
regularly at a rate of between 20 and 100 Pa/s (according to
the estimated pore size), while the surface of the test piece
is under constant observation. In the case of a hollow
cylindrical test piece, rotate it so that all of the surface is
observed; in this case, increase the pressure in steps, each of
from 50 to 500 Pa (according to the estimated pore size),
so that each new pressure value is maintained whilst the
surface is observed during the rotation.
Note the first bubble pressure when a string of bubbles
occurs from one distinct point (or perhaps several distinct
ooints at the same time).
If there is a defect, the first bubble may appear in a zone
remote from the upper surface. In this event, reduce the
pressure and repeat the test after rotating the sample on
its own axis; increase the pressure again incrementally.
NOTES
1 The test piece shall be impregnated to ensure the saturation of its open porosity. A vacuum impregnation in accordance with the requirements given in IS0 2738 is recommended.
2 When a determination is repeated on the same sample, it is necessary fo re-impregnate the sample totally before retesting.
3 It is important that the test piece be properly sealed in the apparatus. If bubbles emerge from the proximity of the seals, the result shall be ignored and the fest repeated with improved seals.
4 When’ the test piece is composed of a layer of fine pores supported on a base of coarser pores, the bubble test pore size characterizing the material is that of the fine pore layer. The test piece shall be tested in such a way that the bubbles appear at the surface of the fine pore layer.
5 By agreement between user and supplier, pore sizes correspond- ing to other bubbling conditions may be determined as indicated in clause 4, note 2.
7 EXPRESSION OF RESULTS
Calculate the bubble test pore size, using the formula in
clause 4. Report the arithmetical mean of three determi-
nations rounded to the nearest 5 %.
8 TEST REPORT
The test report shall include the following information :
a) reference to this International Standard;
b) all details necessary for identification of the test
sample;
c) the liquid used;
d) the rate of pressure increase;
e) the position of the first bubble;
f) the result obtained;
g) all operations not specified by this International
Standard, or regarded as optional;
h) details of any occurrence which may have affected
the result.
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