1、Designation: D4404 10Standard Test Method forDetermination of Pore Volume and Pore Volume Distributionof Soil and Rock by Mercury Intrusion Porosimetry1This standard is issued under the fixed designation D4404; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of the porevolume and the pore volu
3、me distributions of soil and rock bythe mercury intrusion porosimetry method. The range ofapparent diameters of pores for which this test method isapplicable is fixed by the operating pressure range of thetesting instrument. This range is typically between apparentpore entrance diameters of about 10
4、0 m and 2.5 nm (0.0025m). Larger pores must be measured by another method.1.2 Mercury intrusion porosimetry is useful only for mea-suring pores open to the outside of a soil or rock fragment;mercury intrusion porosimetry will not give the volume of anypores completely enclosed by surrounding solids.
5、 This testmethod will give only the volume of intrudable pores that havean apparent diameter corresponding to a pressure within thepressurizing range of the testing instrument.1.3 Mercury intrusion may involve the application of highpressures to the specimen. This may result in a temporary orpermane
6、nt alteration or both in the pore geometry. Generally,soils and rocks are composed of comparatively strong solidsand are less subject to these alterations than certain othermaterials. However, the possibility remains that the use of thistest method may alter the natural pore volume distribution that
7、is being measured.1.4 All observed and calculated values shall conform to theguidelines for significant digits and rounding established inPractice D6026.1.5 WarningMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervous system, kidney and liver
8、 damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury-containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/mercury/faq.htm) for additio
9、nal informa-tion. Users should be aware that selling mercury or mercury-containing products or both into your state may be prohibitedby state law.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 This standard does not pur
10、port to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.For specific precaution statements,
11、 see Section 8.2. Referenced Documents2.1 ASTM Standards:2D653 Terminology Relating to Soil, Rock, and ContainedFluidsD3740 Practice for Minimum Requirements for AgenciesEngaged in Testing and/or Inspection of Soil and Rock asUsed in Engineering Design and ConstructionD6026 Practice for Using Signif
12、icant Digits in GeotechnicalData3. Terminology3.1 For definitions of terms used in the test method, refer toTerminology D653.3.2 Definitions of Terms Specific to This Standard:3.2.1 apparent pore diameterthe diameter of a pore that isassumed to be cylindrical and that is intruded at a pressure, P,gi
13、ven by the equation in 13.1.3.2.2 inter-specimen poresthose pores between particleswhen they are packed together and that are intruded during thetest.3.2.3 intra-specimen poresthose pores lying within theexterior outlines of the individual soil and rock fragments.3.2.4 intruded pore volumethe correc
14、ted volume of mer-cury intruded during the test.1This test method is under the jurisdiction ofASTM Committee D18 on Soil andRock and is the direct responsibility of Subcommittee D18.06 on Physical-ChemicalInteractions of Soil and Rock.Current edition approved May 1, 2010. Published June 2010. Origin
15、allyapproved in 1984. Last previous edition approved in 1998 as D440484(2004).DOI: 10.1520/D4404-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Do
16、cument Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Summary of Test Method4.1 When a liquid does not wet a porous solid, it will
17、notenter the pores in the solid by capillary action. The non-wettingliquid (mercury in this test method) can be forced into the poresby the application of external pressure. The size of the poresthat are intruded is inversely proportional to the appliedpressure. When a cylindrical pore model is assu
18、med, therelationship between pressure and size is given as follows:d 524gcosu!/P (1)where:d = apparent pore diameter being intruded,g = surface tension of the mercury,u = contact angle between the mercury and the pore wall,andP = absolute pressure causing the intrusion.Any set of convenient and comp
19、atible units may be used.4.2 The volume of the intruded pores is determined bymeasuring the volume of mercury forced into them at variouspressures. A single determination involves increasing thepressure, either continuously or step-wise, and recording themeasured intruded volume at various pressures
20、.5. Significance and Use5.1 This test method is intended for use in determining thevolume and the volume distribution of pores in soil and rockwith respect to the apparent diameter of the entrances of thepores. In general, both the size and volume of the pores affectsthe performance of soil and rock
21、. Thus, the pore volumedistribution is useful in understanding soil and rock perfor-mance and in identifying a material that can be expected toperform in a particular manner (1, 2).35.2 The intrusion process to determine the volume of a poreproceeds from the outside of a specimen toward its center.C
22、omparatively large interior pores can exist that have smalleroutside openings as the only means of access. Mercuryintrusion porosimetry will incorrectly register the entire vol-ume of these “ink-bottle” pores as having the apparent diam-eter of the smaller access pores. In a test specimen, exteriors
23、pecimen pores can exist in addition to intra-specimen pores(see Section 3 for definitions). The inter-fragment pores willvary in size and volume depending on the size and shape of thesoil or rock fragments and on the manner in which thefragments are packed together. It is possible that some exterior
24、specimen pores can have the same apparent diameter as someintra-specimen pores. When this occurs, this test methodcannot distinguish between them. Thus, the test method yieldsan intruded pore volume distribution that is in part dependentupon the packing of multifragment specimens. However, mostsoils
25、 and rocks have intra-fragment pores much smaller thanthe inter-fragment pores. This situation leads to a bi-modalpore size distribution and the distinction between the twoclasses of pores can then be made (see Figs. 1 and 2).NOTE 1Notwithstanding the statement on precision and bias con-tained in th
26、is test method: The precision of this test method is dependenton the competence of the personnel performing it, and the suitability of theequipment and facilities used.Agencies which meet the criteria of PracticeD3740 are generally considered capable of competent and objectivetesting. Users of this
27、test method are cautioned that compliance withPractice D3740 does not in itself assure reliable testing. Reliable testingdepends on several factors; Practice D3740 provides a means of evaluat-ing some of those factors.6. Apparatus6.1 Mercury Intrusion PorosimeterThis shall be equippedwith a specimen
28、 holder capable of containing one or severalsoil or rock fragments. This specimen holder is frequentlycalled a penetrometer. The porosimeter shall have a means ofsurrounding the test specimen with mercury at a low pressure,3The boldface numbers in parentheses refer to the list of references appended
29、 tothis standard.FIG. 1 Example of Cumulative Pore Volume Distribution PlotD4404 102a pressure generator to cause intrusion, pressure transducers,capable of measuring the intruding pressure with an accuracyof at least 61 % throughout the range of pressures over whichthe pores of interest are being i
30、ntruded, and a means ofmeasuring intruded mercury volumes to an accuracy of at least61mm3(6103cm3).6.2 Vacuum Pump, if not part of the porosimeter, to evacuatethe specimen holder.6.3 Analytical Balance, with an accuracy of at least 6107kg (60.1 mg).6.4 Flume Hood7. Reagent7.1 Triple-Distilled Mercur
31、y.7.2 Other grades or amalgams may be used, provided it isfirst ascertained that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.7.3 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is
32、 intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.8. Safety Precautions8.1 Mercury is a hazardous substance that can cause illnessand death.NOTE 2Mercury is found in several chemical
33、 forms, such as: elemen-tal, inorganic, and organic:A) Elemental Mercury: Elemental mercury, also referred to as metallicmercury, is a shiny, silver-white, odorless liquid. Elemental mercuryreadily evaporates at room temperature to form a colorless, odorless gas.In an enclosed space, even a relative
34、ly small amount of mercury can resultin the accumulation of a very high level of mercury vapor in indoor air.Therefore, exposure via inhalation of elemental mercury is a particularconcern when mercury is spilled in laboratories or in other enclosed areas.B) Inorganic Mercury: Mercury combines with o
35、ther elements, such aschlorine, sulfur, or oxygen, to form inorganic mercury compounds or“salts,” which are usually in the form of white powders or crystals.Inorganic mercury does not readily evaporate and is not easily inhaled;however inorganic mercury can be absorbed across the gastrointestinaltra
36、ct and the surface of the skin. Therefore, ingestion and skin contact canresult in exposure.C) Organic Mercury: Mercury also combines with carbon to makeorganic mercury compounds. The most common form is methyl mercury,which is produced mainly by small organisms in the water, soil, andsediment. Incr
37、easing emissions of mercury into the environment canincrease the levels of methyl mercury that these small organisms make.The most significant source of human exposure to organic mercury isthrough diet, particularly from fish products. Since organic mercury iseasily absorbed through the gastrointest
38、inal tract and through the skin,ingestion and skin contact can result in exposure.8.2 Store mercury in closed containers to control its evapo-ration and use only in conjunction with a flume hood in awell-ventilated room.8.3 Mercury can also be absorbed through the skin, so avoiddirect contact. Wash
39、hands immediately after any operationinvolving mercury; the use of mercury approved gloves isadvocated.8.4 Exercise extreme care to avoid spilling mercury. Cleanup any spills immediately using procedures recommendedexplicitly for mercury.8.5 Handle intruded specimens with great care and disposeof in
40、 a safe and environmentally acceptable manner immedi-ately after completion of the test (See Note 3).NOTE 3USEPA conditionally exempts small quantity generatorsFIG. 2 Example of Differential Pore Volume Distribution PlotD4404 103(CESQC). Small quantity generators (CESQC) generate 100 kg or less perm
41、onth of hazardous waste, or 1 kg or less per month of acutely hazardouswaste. Requirements for CESQGs include (see also 40 CFR 261.54):CESQGs must identify all the hazardous waste.CESQGs must identify all the hazardous waste generated.CESQGs may not accumulate more than 1 000 kg of hazardous wasteat
42、 any time.CESQGs must ensure that hazardous waste is delivered to a person orfacility that is authorized to manage it.9. Sampling, Test Specimens, and Test Units9.1 The sample from which the test specimen is drawn shallbe representative of the soil or rock. The test specimen shall beas large as prac
43、ticable considering the test apparatus.NOTE 4A minimum of 3 specimens should be run on samples fromsimilar material. If a statistical analysis of the results is desired, aminimum of 10 specimens is required.NOTE 5Specimen size is limited by the pore-measuring capacity ofthe penetrometer, which is cu
44、rrently (1984) slightly more than 16 387mm.3The small specimen size may prevent the measurement of porosityrepresented by relatively large cracks and fissures in the material.Judgement is required in the application of these measurements to thecharacterization of the soil or rock masses.10. Conditio
45、ning10.1 The ideal preconditioning for the test specimen is anoutgassing or drying procedure such as freeze drying andcritical region drying that removes all foreign fluids from thepores and pore walls of the soil or rock and does not alter thesoil or rock in any way. If possible, the appropriate co
46、mbina-tion of temperature and pressure and the required time ofconditioning shall be experimentally determined for the spe-cific soil or rock under test. This outgassing or drying tech-nique shall then be the one specified and used.10.2 Rock or coarse-grained soil without fines shall beoutgassed in
47、a vacuum at least 1.3 Pa (10 mHg) and at atemperature of 150 C for at least 24 h. Soil containing anyplastic fines requires special drying procedures to avoid alter-ation of pore structure. Freeze drying has been successfullyemployed (3, 4) and is a simple procedure. Critical regiondrying may also b
48、e used (5), but is more complex andexpensive than freeze drying.11. Procedure11.1 Outgas or dry the test specimen in accordance with10.1 or 10.2.11.2 Weigh the outgassed or dried specimen and record thisweight.11.3 Place the outgassed or dried material in the penetrom-eter.NOTE 6When performing the
49、operation described in 11.2 and 11.3,the outgassed or dried material is exposed to the laboratory atmosphereand can readsorb vapors. Thus, this operation should be carried out asrapidly as possible.11.4 Place the penetrometer containing the specimen in thepressure vessel of the porosimeter and evacuate to a pressure ofat least 1.3 Pa (10 mHg).11.5 Fill the penetrometer with mercury by pressurizing tothe minimum pressure greater than 1.3 Pa (10 mHg) that willpromote filling.NOTE 7The pressure required to fill the penetrometer with mercury isalso capable of i
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