ASTM D4284-12
(Test Method)Standard Test Method for Determining Pore Volume Distribution of Catalysts and Catalyst Carriers by Mercury Intrusion Porosimetry
Standard Test Method for Determining Pore Volume Distribution of Catalysts and Catalyst Carriers by Mercury Intrusion Porosimetry
SIGNIFICANCE AND USE
This test method is intended to determine the volume distribution of pores in catalysts and catalyst carriers with respect to the apparent diameter of the entrances to the pores. In general, both the size and volume of pores in a catalyst affect its performance. Thus, the pore volume distribution is useful in understanding a catalyst's performance and in specifying a catalyst that can be expected to perform in a desired manner.
SCOPE
1.1 This test method covers the determination of the pore volume distributions of catalysts and catalyst carriers by the method of mercury intrusion porosimetry. The range of apparent diameters of pores for which it 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 and 0.003 μm (3 nm).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s websitehttp://www.epa.gov/mercury/faq.htmfor additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be prohibited by law.
1.4 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 establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard information is given in Section 8.
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Designation: D4284 − 12
Standard Test Method for
Determining Pore Volume Distribution of Catalysts and
1
Catalyst Carriers by Mercury Intrusion Porosimetry
This standard is issued under the fixed designation D4284; 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 E177Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
1.1 This test method covers the determination of the pore
E456Terminology Relating to Quality and Statistics
volume distributions of catalysts and catalyst carriers by the
E691Practice for Conducting an Interlaboratory Study to
method of mercury intrusion porosimetry. The range of appar-
Determine the Precision of a Test Method
ent diameters of pores for which it is applicable is fixed by the
operant pressure range of the testing instrument. This range is
3. Terminology
typically between apparent pore entrance diameters of about
3.1 Definitions of Terms Specific to This Standard:
100 and 0.003 µm (3 nm).
3.1.1 apparent pore diameter—the diameter of a pore,
1.2 The values stated in SI units are to be regarded as
assumed to be cylindrical, that is intruded at a pressure, P, and
standard. No other units of measurement are included in this
is calculated with Eq 1.
standard.
3.1.2 interparticle pores—those pores that occur between
1.3 WARNING—Mercury has been designated by many
particles when they are packed together and that are intruded
regulatory agencies as a hazardous material that can cause
during the test.
central nervous system, kidney and liver damage. Mercury, or
3.1.3 intraparticle pores—those pores lying within the en-
its vapor, may be hazardous to health and corrosive to
velopesoftheindividualcatalystparticlesandthatareintruded
materials.Cautionshouldbetakenwhenhandlingmercuryand
during the test.
mercury containing products. See the applicable product Ma-
3.1.4 intruded pore volume—the volume of mercury that is
terial Safety Data Sheet (MSDS) for details and EPA’s
intruding into the pores during the test after this volume has
website—http://www.epa.gov/mercury/faq.htm—for addi-
been corrected, if necessary, per 13.3.2.
tional information. Users should be aware that selling mercury
and/or mercury containing products into your state or country
4. Summary of Test Method
may be prohibited by law.
4.1 When a liquid does not wet a porous solid it will not
1.4 This standard does not purport to address all of the
voluntarily enter the pores in the solid by capillary attraction.
safety problems, if any, associated with its use. It is the
The nonwetting liquid (mercury in this test method) must be
responsibility of the user of this standard to establish appro-
forced into the pores by the application of external pressure.
priate safety and health practices and determine the applica-
Thesizeoftheporesthatareintrudedisinverselyproportional
bility of regulatory limitations prior to use. Specific hazard
to the applied pressure. When a cylindrical pore model is
information is given in Section 8.
assumed, the relationship between pressure and size is:
24γ cos θ
~ !
2. Referenced Documents
d 5 (1)
P
2
2.1 ASTM Standards:
where:
d = apparent diameter of the pore being intruded,
1 γ = surface tension of the mercury,
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.01 on Physical- θ = contact angle between the mercury and the solid, and
Chemical Properties.
P = absolute pressure causing the intrusion.
CurrenteditionapprovedMay1,2012.PublishedJuly2012.Originallyapproved
4.2 The volume of the intruded pores is determined by
in 1983. Last previous edition approved in 2007 as D4284–07. DOI: 10.1520/
D4284-12.
measuring the volume of mercury that is forced into them at
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
variouspressures.Asingle-poresizedistributiondetermination
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
involves increasing the pressure, either continuously or step-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. wise, and recording the measured intruded volume.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D4284 − 12
5. Significance and Use of interest are being intruded, and a means of measuring the
intruded mercury volumes with an accuracy of at least 61
5.1 This test method is intended to determine the volume
3 −3 3
mm (610 cm ).
distribution of pores in
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately,ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D4284–07 Designation:D4284–12
Standard Test Method for
Determining Pore Volume Distribution of Catalysts and
1
Catalyst Carriers by Mercury Intrusion Porosimetry
This standard is issued under the fixed designation D4284; 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
1.1 This test method covers the determination of the pore volume distributions of catalysts and catalyst supportscarriers by the
methodofmercuryintrusionporosimetry.Therangeofapparentdiametersofporesforwhichitisapplicableisfixedbytheoperant
pressure range of the testing instrument.This range is typically between apparent pore entrance diameters of about 100 and 0.003
µm (3 nm).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3
1.3 WARNING—Mercury has been designated by many regulatory agencies as a hazardous material that can cause central
nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution
should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet
(MSDS) for details and EPA’s website—http://www.epa.gov/mercury/faq.htm—for additional information. Users should be aware
that selling mercury and/or mercury containing products into your state or country may be prohibited by law.
1.4 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 establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazard information is given in Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 apparent pore diameter—the diameter of a pore, assumed to be cylindrical, that is intruded at a pressure, P, and is
calculated with Eq 1.
3.1.2 interparticle pores—those pores that occur between particles when they are packed together and that are intruded during
the test.
3.1.3 intraparticle pores—thoseporeslyingwithintheenvelopesoftheindividualcatalystparticlesandthatareintrudedduring
the test.
3.1.4 intruded pore volume—the volume of mercury that is intruding into the pores during the test after this volume has been
corrected, if necessary, per 13.3.2.
4. Summary of Test Method
4.1 When a liquid does not wet a porous solid it will not voluntarily enter the pores in the solid by capillary attraction. The
nonwetting liquid (mercury in this test method) must be forced into the pores by the application of external pressure. The size of
the pores that are intruded is inversely proportional to the applied pressure. When a cylindrical pore model is assumed, the
relationship between pressure and size is:
1
This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.01 on Physical-Chemical
Properties.
Current edition approved AprilMay 1, 2007.2012. Published April 2007.July 2012. Originally approved in 1983. Last previous edition approved in 20032007 as
D4284–03.D4284–07. DOI: 10.1520/D4284-07.10.1520/D4284-12.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4284–12
24g~cosu!
d 5 (1)
P
D4284-12_1
where:
d = apparent diameter of the pore being intruded,
g = surface tension of the mercury,
u = contact angle between the mercury and the solid, and
P = absolute pressure causing the intrusion.
4.2 The volume of the intruded pores is determined by measuring the volume of mercury that is forced into them at various
pressures. A single-pore size distribution determination involves incre
...
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