1、Designation: D4404 18Standard 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 40
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 WarningMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andm
8、ercury-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 additional informa-tion. Users should be aware that selling mercury or mercury-containing products or both into your state may be prohibitedby
9、 state law.1.5 UnitsThe values stated in SI units are to be regardedas standard. No other units of measurement are included in thisstandard. Reporting of test results in units other than SI, suchas cgs, shall not be regarded as nonconformance with this testmethod.1.6 All observed and calculated valu
10、es shall conform to theguidelines for significant digits and rounding established inPractice D6026.1.6.1 The procedures used to specify how data are collected/recorded and calculated in this standard are regarded as theindustry standard. In addition, they are representative of thesignificant digits
11、that generally should be retained. The proce-dures used do not consider material variation, purpose forobtaining the data, special purpose studies, or any consider-ations for the users objectives; and it is common practice toincrease or reduce significant digits of reported data to becommensurate wi
12、th these considerations. It is beyond the scopeof these test methods to consider significant digits used inanalysis methods for engineering data.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this stand
13、ard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific precaution statements, see Section 8.1.8 This international standard was developed in accor-dance with internationally recognized principles
14、on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D653 Terminology Relating to Soil, Roc
15、k, and ContainedFluidsD3740 Practice for Minimum Requirements for Agencies1This 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 Feb. 1, 2018.
16、Published March 2018. Originallyapproved in 1984. Last previous edition approved in 2010 as D440410. DOI:10.1520/D4404-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, ref
17、er to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with
18、internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1Engaged in Testing and/or Inspection of Soi
19、l and Rock asUsed in Engineering Design and ConstructionD6026 Practice for Using Significant Digits in GeotechnicalData3. Terminology3.1 For definitions of common technical terms used in thisstandard, refer to Terminology D653.3.2 Definitions of Terms Specific to This Standard:3.2.1 apparent pore di
20、ameterthe diameter of a pore that isassumed to be cylindrical and that is intruded at a pressure, P,given 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 with
21、in theexterior outlines of the individual soil and rock fragments.3.2.4 intruded pore volumethe corrected volume of mer-cury intruded during the test.4. Summary of Test Method4.1 When a liquid does not wet a porous solid, it will notenter the pores in the solid by capillary action. The non-wettingli
22、quid (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. The diameter of the pores filled can be calculatedfrom this applied pressure as described in Section 13, Ca
23、lcu-lations.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.4.2.1 The sa
24、mple is contained in a sample cell frequentlycalled a penetrometer. The sample is contained within a sealedbowl to which a small capillary is attached. The space in thepenetrometer not occupied by the sample is first evacuated andthen filled with mercury. One end of the penetrometer is openand seale
25、d to the pressure system of the instrument. Pressureapplied to the open end of the penetrometer capillary is thenused to force the mercury into the pores, with larger poresfilling at lower applied pressures, and smaller pores filling athigher applied pressures.4.3 Additional information about the po
26、re structure of thematerial may be determined by recording of the extrusionprofile for the sample. This is performed by recording thecumulative quantity of mercury contained within the sample aspressure is reduced, again either continuously or step-wise.4.4 Commercially available instruments include
27、 softwarefor controlling sample evacuation, filling of sample penetrom-eter with mercury, pressurization of the sample according to aprogrammed scheme, allowance for equilibration of thepressure, recording of the pressure and amount of mercuryintruded into the sample, and calculation of summary resu
28、lts.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 r
29、ock. 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 cente
30、r.Comparatively 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, exteri
31、orspecimen pores can exist in addition to intra-specimen pores(see 3.2 for definitions). The inter-fragment pores will vary insize and volume depending on the size and shape of the soil orrock fragments and on the manner in which the fragments arepacked together. It is possible that some exterior sp
32、ecimenpores can have the same apparent diameter as some intra-specimen pores. When this occurs, this test method cannotdistinguish between them. Thus, the test method yields anintruded pore volume distribution that is in part dependentupon the packing of multifragment specimens. However, mostsoils a
33、nd 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). Theintr-fragment pore concentration is shown to the left of theplot; the in
34、ter-fragment concentration is to the right.NOTE 1The quality of the result produced by this standard isdependent on the competence of the personnel performing it, and thesuitability of the equipment and facilities used. Agencies that meet thecriteria of Practice D3740 are generally considered capabl
35、e of competentand objective testing/sampling/inspection/etc. Users of this standard arecautioned that compliance with Practice D3740 does not in itself assurereliable results. Reliable results depend on many factors; Practice D3740provides a means of evaluating some of those factors.6. Apparatus6.1
36、Mercury Intrusion PorosimeterA device equippedwith a specimen 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,a pressure gener
37、ator 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 intruded, and a means ofmeasuring intruded mercury volumes to an accuracy of at least61mm3.6.2 Analyt
38、ical Balance, with an accuracy of at least 6106kg (61 mg), and readable to at least 6107kg (60.1 mg).3The boldface numbers in parentheses refer to the list of references appended tothis standard.D4404 1826.3 Fume HoodA ventilated enclosure designed to limitexposure to hazardous/toxic vapors, fumes,
39、or dust by provid-ing a means to move the air away from the user, preferablyventing it outside.6.4 Thermometric DeviceA thermometric device capableof measuring the temperature range within which the test isbeing performed readable to 0.5C or better and having anaccuracy of at least 61. The thermomet
40、ric device shall bestandardized by comparison to a nationally or internationallytraceable thermometric device and shall include at least onetemperature reading within the range of testing. The thermo-metric device shall be standardized at least once every twelvemonths.6.5 Drying OvenControllable at
41、or above 150 6 10C.7. Reagent7.1 Triple-Distilled Mercury.7.2 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatFIG. 1 Example of Cumulative Pore Volume Distribution PlotFIG. 2 Example of Differential Pore Volume Distribution PlotD440
42、4 183all reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.4Other grades or amalgamsmay be used, provided it is first ascertained that the reagent isof sufficiently high purity to permit its use witho
43、ut lesseningthe accuracy of the determination.8. Safety Precautions8.1 WarningMercury has been designated by many regu-latory agencies as a hazardous material that can cause seriousmedical issues. Mercury, or its vapor, has been demonstrated tobe hazardous to health and corrosive to materials. Cauti
44、onshould be taken when handling mercury and mercury contain-ing products. See the applicable Safety Data Sheet (SDS) foradditional information. Users should be aware that sellingmercury and/or mercury containing products into your state orcountry may be prohibited by law (see Note 2).NOTE 2Mercury i
45、s found in several chemical forms, such as:elemental, 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 enclo
46、sed space, even a relatively 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.Vapor levels can be
47、 limited through temperature control of and fresh airflow through the laboratory space where the analysis is performed. Manylaboratories are maintained at or below 293 K (20C), with forced air flowthrough the area either through use of exhaust fans or a continuously-operating fume hood.(B) Inorganic
48、 Mercury: Mercury combines with other 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 absorb
49、ed across the gastrointestinaltract 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. Increasing 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 pro
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