ASTM D4404-84(2004)
(Test Method)Standard Test Method for Determination of Pore Volume and Pore Volume Distribution of Soil and Rock by Mercury Intrusion Porosimetry
Standard Test Method for Determination of Pore Volume and Pore Volume Distribution of Soil and Rock by Mercury Intrusion Porosimetry
SIGNIFICANCE AND USE
This test method is intended for use in determining the volume and the volume distribution of pores in soil and rock with respect to the apparent diameter of the entrances of the pores. In general, both the size and volume of the pores affects the soil or rock performance. Thus, the pore volume distribution is useful in understanding soil and rock performance and in identifying a material that can be expected to perform in a particular manner (1, 2).4
SCOPE
1.1 This test method covers the determination of the pore volume and the pore volume distributions of soil and rock by the mercury intrusion porosimetry method. The range of apparent diameters of pores for which this test method is applicable is fixed by the operant pressure range of the testing instrument. This range is typically between apparent pore entrance diameters of about 100 [mu]m and 2.5 nm (0.0025 [mu]m). Larger pores must be measured by another method.
1.2 Mercury intrusion porosimetry is useful only for measuring pores open to the outside of a soil or rock fragment; mercury intrusion porosimetry will not give the volume of any pores completely enclosed by surrounding solids. This test method will give only the volume of intrudable pores that have an apparent diameter corresponding to a pressure within the pressurizing range of the testing instrument.
1.3 The intrusion process proceeds from the outside of a fragment toward its center. Comparatively large interior pores can exist that have smaller pores as the only means of access. Mercury intrusion porosimetry will incorrectly register the entire volume of these "ink-bottle" pores as having the apparent diameter of the smaller access pores. In a test sample, inter-fragment pores can exist in addition to intra-fragment pores (see Section 3 for definitions). The inter-fragment pores will vary in size and volume depending on the size and shape of the soil or rock fragments and on the manner in which the fragments are packed together. It is possible that some inter-fragment pores can have the same apparent diameter as some intra-fragment pores. When this occurs this test method cannot distinguish between them. Thus, the test method yields an intruded pore volume distribution that is in part dependent upon the packing of multifragment samples. However, most soils and rocks have intra-fragment pores much smaller than the inter-fragment pores. This situation leads to a bi-modal pore size distribution and the distinction between the two classes of pores can then be made (see Figs. 1 and 2).
1.4 Mercury intrusion may involve the application of high pressures to the sample. This may result in a temporary, or permanent, or temporary and permanent alteration in the pore geometry. Generally, soils and rocks are composed of comparatively strong solids and are less subject to these alterations than certain other materials. However, the possibility remains that the use of this test method may alter the natural pore volume distribution that is being measured.
1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precaution statements, see Section 8.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4404–84 (Reapproved 2004)
Standard Test Method for
Determination of Pore Volume and Pore Volume Distribution
of Soil and Rock by Mercury Intrusion Porosimetry
This standard is issued under the fixed designation D4404; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.4 Mercury intrusion may involve the application of high
pressures to the sample. This may result in a temporary, or
1.1 This test method covers the determination of the pore
permanent, or temporary and permanent alteration in the pore
volume and the pore volume distributions of soil and rock by
geometry. Generally, soils and rocks are composed of com-
the mercury intrusion porosimetry method. The range of
paratively strong solids and are less subject to these alterations
apparent diameters of pores for which this test method is
than certain other materials. However, the possibility remains
applicable is fixed by the operant pressure range of the testing
that the use of this test method may alter the natural pore
instrument. This range is typically between apparent pore
volume distribution that is being measured.
entrance diameters of about 100 µm and 2.5 nm (0.0025 µm).
1.5 This standard does not purport to address all of the
Larger pores must be measured by another method.
safety concerns, if any, associated with its use. It is the
1.2 Mercury intrusion porosimetry is useful only for mea-
responsibility of the user of this standard to consult and
suring pores open to the outside of a soil or rock fragment;
establish appropriate safety and health practices and deter-
mercury intrusion porosimetry will not give the volume of any
mine the applicability of regulatory limitations prior to use.
pores completely enclosed by surrounding solids. This test
For specific precaution statements, see Section 8.
methodwillgiveonlythevolumeofintrudableporesthathave
an apparent diameter corresponding to a pressure within the
2. Referenced Documents
pressurizing range of the testing instrument.
2.1 ASTM Standards:
1.3 The intrusion process proceeds from the outside of a
C699 MethodforChemical,MassSpectrometric,andSpec-
fragment toward its center. Comparatively large interior pores
trochemicalAnalysis of, and Physical Tests on, Beryllium
can exist that have smaller pores as the only means of access.
Oxide Powder
Mercury intrusion porosimetry will incorrectly register the
entire volume of these “ink-bottle” pores as having the
3. Terminology
apparentdiameterofthesmalleraccesspores.Inatestsample,
3.1 Definitions:
inter-fragment pores can exist in addition to intra-fragment
3.1.1 apparent pore diameter—thediameterofaporethatis
pores (see Section 3 for definitions). The inter-fragment pores
assumed to be cylindrical and that is intruded at a pressure, P,
will vary in size and volume depending on the size and shape
given by the equation in 4.1.
of the soil or rock fragments and on the manner in which the
3.1.2 inter-fragment pores—those pores between fragments
fragments are packed together. It is possible that some inter-
when they are packed together and that are intruded during the
fragment pores can have the same apparent diameter as some
test.
intra-fragmentpores.Whenthisoccurs,thistestmethodcannot
3.1.3 intra-fragment pores—those pores lying within the
distinguish between them. Thus, the test method yields an
exterior outlines of the individual soil and rock fragments.
intruded pore volume distribution that is in part dependent
3.1.4 intruded pore volume—the corrected volume of mer-
upon the packing of multifragment samples. However, most
cury intruded during the test.
soils and rocks have intra-fragment pores much smaller than
the inter-fragment pores. This situation leads to a bi-modal
4. Summary of Test Method
pore size distribution and the distinction between the two
4.1 When a liquid does not wet a porous solid, it will not
classes of pores can then be made (see Fig. 1 and Fig. 2).
entertheporesinthesolidbycapillaryaction.Thenon-wetting
liquid(mercuryinthistestmethod)canbeforcedintothepores
ThistestmethodisunderthejurisdictionofASTMCommitteeD18onSoiland
RockandisthedirectresponsibilityofSubcommitteeD18.06onPhysical-Chemical For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Interactions of Soil and Rock. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
CurrenteditionapprovedJuly1,2004.PublishedJuly2004.Originallyapproved Standards volume information, refer to the standard’s Document Summary page on
´1
in 1984. Last previous edition approved in 1998 as D4404-84 (1998) . DOI: the ASTM website.
10.1520/D4404-84R04. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4404–84 (2004)
FIG. 1 Example of Cumulative Pore Volume Distribution Plot
FIG. 2 Example of Differential Pore Volume Distribution Plot
by the application of external pressure. The size of the pores Any set of convenient and compatible units may be used.
that are intruded is inversely proportional to the applied 4.2 The volume of the intruded pores is determined by
pressure. When a cylindrical pore model is assumed, the measuring the volume of mercury forced into them at various
relationship between pressure and size is given as follows: pressures. A single determination involves increasing the
pressure, either continuously or step-wise, and recording the
d 524g~cosu!/P (1)
measured intruded volume at various pressures.
where:
d = apparent pore diameter being intruded, 5. Significance and Use
g = surface tension of the mercury,
5.1 This test method is intended for use in determining the
u = contact angle between the mercury and the pore wall,
volume and the volume distribution of pores in soil and rock
and
with respect to the apparent diameter of the entrances of the
P = absolute pressure causing the intrusion.
pores. In general, both the size and volume of the pores affects
D4404–84 (2004)
the soil or rock performance. Thus, the pore volume distribu- mined for the specific soil or rock under test. This outgassing
tion is useful in understanding soil and rock performance and or drying technique shall then be the one specified and used.
in identifying a material that can be expected to perform in a 10.2 Where the procedure described in 10.1 is not practical,
particular manner (1, 2). rock or coarse-grained soil without fines shall be outgassed in
a vacuum at least 1.3 Pa (10 µmHg) and at a temperature of
6. Apparatus
150°C for at least 24 h. Soil containing any plastic fines
6.1 Mercury Intrusion Porosimeter—Thisshallbeequipped requires special drying procedures to avoid alteration of pore
with a sample holder capable of containing one or several soil
structure. Freeze drying has been successfully employed (3, 4)
or rock fragments. This sample holder is frequently called a and is a simple procedure. Critical region drying may also be
penetrometer.Theporosimetershallhaveameansofsurround-
used (5), but is more complex and expensive than freeze
ing the test specimen with mercury at a low pressure, a drying.
pressure generator to cause intrusion, pressure transducers,
11. Procedure
capable of measuring the intruding pressure with an accuracy
of at least 61% throughout the range of pressures over which 11.1 Outgas or dry the test specimen in accordance with
the pores of interest are being intruded, and a means of 10.1 or 10.2.
measuringintrudedmercuryvolumestoanaccuracyofatleast 11.2 Weigh the outgassed or dried specimen and record this
3 −3 3
61mm (610 cm ). weight.
6.2 Vacuum Pump,ifnotpartoftheporosimeter,toevacuate 11.3 Place the outgassed or dried material in the penetrom-
the sample holder. eter.
−7
6.3 Analytical Balance, with an accuracy of at least 610
NOTE 2—When performing the operation described in 11.2 and 11.3,
kg (60.1 mg).
the outgassed or dried material is exposed to the laboratory atmosphere
and can readsorb vapors. Thus, this operation should be carried out as
7. Reagent
rapidly as possible.
7.1 Triple-Distilled Mercury.
11.4 Place the penetrometer containing the sample in the
appropriate chamber of the porosimeter, following the manu-
8. Safety Precautions
facturer’sinstructions,andevacuatetoapressureofatleast1.3
8.1 Mercury is a hazardous substance that can cause illness
Pa (10 µmHg).
and death. Store mercury in closed containers to control its
11.5 Fillthepenetrometerwithmercury,inaccordancewith
evaporation and use only in well-ventilated rooms. Mercury
the manufacturer’s instructions, by pressurizing to some suit-
can also be absorbed through the skin, so avoid direct contact.
ably low pressure.
Wash hands immediately after any operation involving mer-
NOTE 3—Thepressurerequiredtofillthepenetrometerwithmercuryis
cury; the use of gloves is advocated. Exercise extreme care to
also capable of intruding sufficiently large pores of both the inter- and
avoid spilling mercury. Clean up any spills immediately using
intra-fragment classes. Thus, the process can intrude some pores and the
procedures recommended explicitly for mercury. Handle in-
volume distribution of these pores cannot subsequently be determined.
truded samples with great care and dispose of in a safe and
This fact should be recognized, and where possible, a filling pressure
environmentally acceptable manner immediately after comple-
should be selected that will not intrude pores in the diameter range of
tion of the test.
interest.
11.6 Place the filled penetrometer in the pressure vessel of
9. Sampling, Test Specimens, and Test Units
the porosimeter and prepare the instrument for pressurization
9.1 The material from which the test sample is drawn shall
and intrusion readings in accordance with the manufacturer’s
berepresentativeofthesoilorrock.Thetestsampleshallbeas
instructions.
large as practicable considering the test apparatus.
11.7 Raise the pressure, either continuously or incremen-
NOTE 1—Sample size is limited by the pore-measuring capacity of the tally, and record both the absolute pressure and the volume of
penetrometer, which is currently (1984) slightly more than 1 cm . The
intruded mercury until the maximum pressure of interest is
small sample size may prevent the measurement of porosity represented
reached.
by relatively large cracks and fissures in the material. Judgement is
NOTE 4—Whenraisingthepressureincrementally,thepressureshallbe
required in the application of these measurements to the characterization
maintained during the pause and not allowed to decrease.
of the soil or rock masses.
NOTE 5—When testing some materials, the time required to achieve
10. Conditioning intrusion equilibrium will not be the same at all pressures. Often the
equilibrium time is appreciably longer at pressures that cause an abrupt
10.1 The ideal preconditioning for the test specimen is an
and large increase in intruded volume. Failure to record the equilibrium
outgassing or drying procedure that removes all foreign sub-
intrusionmayresultinsomeoftheporevolumebeingincorrectlyassigned
stances from the pores and pore walls of the soil or rock and
to smaller pore diameters.The extent to which this may be a problem can
does not alter the soil or rock in any way. If possible, the
be assessed by conducting two tests, each at a different pressure increase
appropriate combination of temperature and pressure and the rate, and comparing the results.
NOTE 6—Use of the equation in 4.1 requires the absolute pressure, P.
required time of conditioning shall be experimentally deter-
Withsomeinstrumentsitmaynotbepossibletoreadtheabsolutepressure
directly. In this case, the gage pressure shall be recorded at each step, and
the absolute pressures subsequently calculated.
The boldface numbers in parentheses refer to the list of references appended to
this standard. NOTE 7—The choice of pressure intervals at which data are to be
D4404–84 (2004)
recordedislefttothejudgmentoftheoperator.Normally,atleast10to15
ofmercuryhasbeenmeasuredonavarietyofsolidsbyseveral
intervals will be required to adequately define the pore volume distribu-
differenttechniques;referencestosomeofthesemeasurements
tion. In selecting these pressure intervals, a rough idea of the expected
are given in Appendix X1. This appendix also lists references
distribution is helpful, since the pressure interval can be larger in regions
for several methods of contact-angle measurement that have
where little or no intrusion occurs and should be smaller in regions where
been found useful. The ideal value for reducing the data is the
a large volume of intrusion is expected. It is not necessary to continue the
one that has been determined for the material under test. If
processuptothemaximumpressurizingcapabilityoftheinstrumentifall
of the pores of interest in a particular test specimen have been intruded at directmeasurementisimpractical,theuseofanassumedvalue
a lesser pressure.
is customary. If mercury intrusion is being used for the
comparison of similar materials for quality control purposes,
11.8 Upon completion of the pressuring cycle, reduce the
then an assumed value is satisfactory; however, when different
pressure and disassemble and clean the instrument in accor-
materialsarebeingcompared,theassumptionofasinglevalue
dance with the manufacturer’s instructions.
for the contact angle may lead to errors.
12. Blank Test for Corrections
13.3 Thenextstepinthecalculationsisthecorrectionofthe
12.1 An intrusion test on a nonporous sample is required to intruded volume readings. Corrections fall into two categories:
obtain values to use in correcting intrusion data for compress-
low-pressure corrections and high-pressure corrections.
ibilities and temperature changes.
13.3.1 Low-pressure corrections account for the fact that
12.2 Selectanonporousmaterialthathasapproximatelythe
part of the apparent intrusion recorded at the lowest pressures
same compressibility and bulk volume as the soil or rock
is actually the compression of the air trapped in the penetrom-
sample that is to be tested.
eter when it was filled with mercury. This correction is
12.3 Test the nonporous sample in exactly the same manner
important only when the distribution of large pores must be
as outlined in Section 11. Raise the pressure in the same steps
measured accurately. When large pores are not of interest
used for the soil or rock tests to ensure that temperature
(pores larger than about 50-µm dia
...
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