ASTM D4567-19
(Test Method)Standard Test Method for Single-Point Determination of Specific Surface Area of Catalysts and Catalyst Carriers Using Nitrogen Adsorption by Continuous Flow Method
Standard Test Method for Single-Point Determination of Specific Surface Area of Catalysts and Catalyst Carriers Using Nitrogen Adsorption by Continuous Flow Method
SIGNIFICANCE AND USE
5.1 This test method is useful for determining the specific surface area of catalysts and catalyst carriers for material specifications, manufacturing control, and research and development in the evaluation of catalysts.
SCOPE
1.1 This test method covers the single-point determination of the surface area of catalysts and catalyst carriers that exhibit Type II or Type IV nitrogen adsorption isotherms using a nitrogen-helium flowing gas mixture. This test method is applicable for the determination of total surface areas from 0.1 to 300 m2, where rapid surface area determinations are desired.
1.2 Because the single-point method uses an approximation of the BET equation, the multipoint BET method (Test Method D3663) is preferred to the single-point method.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to consult and establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:D4567 −19
Standard Test Method for
Single-Point Determination of Specific Surface Area of
Catalysts and Catalyst Carriers Using Nitrogen Adsorption
1
by Continuous Flow Method
This standard is issued under the fixed designation D4567; 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 D3766Terminology Relating to Catalysts and Catalysis
E177Practice for Use of the Terms Precision and Bias in
1.1 This test method covers the single-point determination
ASTM Test Methods
ofthesurfaceareaofcatalystsandcatalystcarriersthatexhibit
E456Terminology Relating to Quality and Statistics
Type II or Type IV nitrogen adsorption isotherms using a
E691Practice for Conducting an Interlaboratory Study to
nitrogen-helium flowing gas mixture. This test method is
Determine the Precision of a Test Method
applicable for the determination of total surface areas from 0.1
2
to300m ,whererapidsurfaceareadeterminationsaredesired.
3. Terminology
1.2 Because the single-point method uses an approximation
3.1 Definitions—See Terminology D3766.
oftheBETequation,themultipointBETmethod(TestMethod
D3663) is preferred to the single-point method.
3.2 Symbols:
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
−20 2
A = cross-sectional area of nitrogen, 16.2×10 m .
cs
standard.
C = integrator counts.
I
T
1.4 This standard does not purport to address all of the
C a = integrator counts corrected for ambient temperature.
I
P
safety concerns, if any, associated with its use. It is the C a = integrator counts corrected for ambient pressure.
I
23
N = Avogadro’s number, 6.02×10 , molecules/mole.
responsibility of the user of this standard to consult and
P = partial pressure of nitrogen, torr.
establish appropriate safety, health, and environmental prac-
P = ambient pressure, torr.
tices and determine the applicability of regulatory limitations a
P = saturated equilibrium vapor pressure of liquid
prior to use. o
nitrogen, torr.
1.5 This international standard was developed in accor-
3
R = gas constant, 82.1 cm atm/K mole.
dance with internationally recognized principles on standard-
T = ambient temperature, K.
a
ization established in the Decision on Principles for the
V = volume of nitrogen adsorbed at ambient temperature
Development of International Standards, Guides and Recom-
3
and pressure, cm .
mendations issued by the World Trade Organization Technical
W = tare of sample cell, g.
1
Barriers to Trade (TBT) Committee.
W = sample mass+tare of sample cell after analysis, g.
2
W = mass of sample, g.
s
2. Referenced Documents
2
2.1 ASTM Standards:
4. Summary of Test Method
D3663Test Method for Surface Area of Catalysts and
4.1 The sample is degassed by heating in a flow of inert gas
Catalyst Carriers
to remove adsorbed vapors from the surface. The sample is
then immersed in a liquid nitrogen bath causing adsorption of
nitrogen from a flowing mixture of a fixed concentration of
1
This test method is under the jurisdiction of Committee D32 on Catalysts and
nitrogeninhelium.Whenadsorptioniscomplete,thesampleis
is the direct responsibility of Subcommittee D32.01 on Physical-Chemical Proper-
ties.
allowed to warm to room temperature causing desorption,
Current edition approved July 1, 2019. Published August 2019. Originally
whichresultsinanincreaseinthenitrogenconcentrationinthe
approved in 1986. Last previous edition approved in 2013 as D4567–03(2013).
flowing mixture. The quantity of nitrogen gas desorbed is
DOI: 10.1520/D4567-19.
2
determined by sensing the change in thermal conductivity.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.2 Calculation of the surface area is based on a modified
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. form of the BET equation.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4567−19
FIG. 1 Apparatus
5. Significance and Use 6.1.4 Equilibration Paths—The apparatus will have at least
two equilibration paths, selected by a selector valve or a
5.1 This test method is useful for determining the specific
combination of valves, between the sample cell and the down
surface area of catalysts and catalyst carriers for materi
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D4567 − 03 (Reapproved 2013) D4567 − 19
Standard Test Method for
Single-Point Determination of Specific Surface Area of
Catalysts and Catalyst Carriers Using Nitrogen Adsorption
1
by Continuous Flow Method
This standard is issued under the fixed designation D4567; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number 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 single-point determination of the surface area of catalysts and catalyst carriers that exhibit Type
II or Type IV nitrogen adsorption isotherms using a nitrogen-helium flowing gas mixture. This test method is applicable for the
2
determination of total surface areas from 0.1 to 300 m , where rapid surface area determinations are desired.
1.2 Because the single-point method uses an approximation of the BET equation, the multipoint BET method (Test Method
D3663) is preferred to the single-point method.
NOTE 1—This is particularly true when testing microporous materials.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of whoever uses the user of this standard to consult and establish appropriate safety safety, health, and healthenvironmental
practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D3663 Test Method for Surface Area of Catalysts and Catalyst Carriers
D3766 Terminology Relating to Catalysts and Catalysis
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—See Terminology D3766.
3.2 Symbols:
−20 2
A = cross-sectional area of nitrogen, 16.2 × 10 m .
cs
C = integrator counts.
I
T
C a = integrator counts corrected for ambient temperature.
I
P
C a = integrator counts corrected for ambient pressure.
I
23
N = Avogadro’s number, 6.02 × 10 , molecules/mole.
P = partial pressure of nitrogen, torr.
P = ambient pressure, torr.
a
1
This test method is under the jurisdiction of Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.01 on Physical-Chemical Properties.
Current edition approved April 1, 2013July 1, 2019. Published August 2013August 2019. Originally approved in 1986. Last previous edition approved in 20082013 as
D4567 – 03(2008).(2013). DOI: 10.1520/D4567-03R13.10.1520/D4567-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@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 ----------------------
D4567 − 19
FIG. 1 Apparatus
P = saturated equilibrium vapor pressure of liquid nitrogen, torr.
o
3
R = gas constant, 82.1 cm atm/K mole.
T = ambient temperature, K.
a
3
V = volume of nitrogen adsorbed at ambient temperature and pressure, cm .
W = tare of sample cell, g.
1
W = sample mass + tare of sample cell after analysis, g.
2
W = mass of sample, g.
s
4. Summary of Test Method
4.1 The sample is degassed by heating in a flow of inert gas to remove adsorbed vapors from the surface. The sample is then
immersed in a liquid nitrogen bath causing adsorption of nitrogen from a flowing mixture of a fixed concentration of nitrogen in
helium. When adsorption is complete, the sample is allowed to warm to room temperature causing desorption, which results in an
increase in the nitrogen concentration in the flowing mixture. The quantity of nitrogen gas desorbed is determined by sensing the
change in thermal conductivity.
4.2 Calculation of the surface area is based
...
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