ASTM D3663-20

Standard Test Method for Surface Area of Catalysts and Catalyst Carriers

ABSTRACT
This test method establishes the standard procedure for determining the surface areas of catalyst and catalyst carriers that have Type II or IV nitrogen adsorption isotherms, and specified minimum area. A volumetric measuring system is used to obtain at least four data points which fit on the linear BET line. The surface area of a catalyst or catalyst carrier is determined by measuring the volume of nitrogen gas adsorbed at various low-pressure levels by the catalyst sample. Pressure differentials caused by introducing the catalyst surface area to a fixed volume of nitrogen in the test apparatus are measured and used to calculate BET surface area.
SCOPE
1.1 This test method covers the determination of surface areas of catalyst and catalyst carriers that have Type II or IV nitrogen adsorption isotherms, and at least 1 m2/g of area. A volumetric measuring system is used to obtain at least four data points which fit on the linear BET2 equation line.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.3 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 establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

General Information

• Status: Published
• Publication Date: 30-Sep-2020
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.01 - Physical-Chemical Properties

Standards Content (Sample)

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: D3663 − 20
Standard Test Method for
1
Surface Area of Catalysts and Catalyst Carriers
This standard is issued under the fixed designation D3663; 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 3.2 Definitions:
3.2.1 surface area of a catalyst, n—the total probe acces-
1.1 This test method covers the determination of surface
siblesurfaceofthecatalyst;itisexpressedinsquaremetresper
areas of catalyst and catalyst carriers that have Type II or IV
2
gram.
nitrogen adsorption isotherms, and at least 1 m /g of area. A
volumetricmeasuringsystemisusedtoobtainatleastfourdata
3.3 Symbols:
2
points which fit on the linear BET equation line.
1.2 Units—The values stated in SI units are to be regarded
P = initial helium pressure, torr
H
as standard. The values given in parentheses after SI units are 1
P = helium pressure after equilibration, torr
H
2
provided for informationonlyandarenotconsideredstandard.
T = temperatureofmanifoldatinitialheliumpressure,
H
1
1.3 This standard does not purport to address all of the
°C
safety concerns, if any, associated with its use. It is the
T = temperature of manifold after equilibration, °C
H
2
responsibility of the user of this standard to establish appro-
P = initial N pressure, torr
1 2
priate safety, health, and environmental practices and deter- T = manifold temperature at initial N pressure, K
1 2
mine the applicability of regulatory limitations prior to use. T ' = manifold temperature at initial N pressure, °C
1 2
P = pressure after equilibration, torr
1.4 This international standard was developed in accor-
2
P = liquid nitrogen vapor pressure, torr
dance with internationally recognized principles on standard- 0
T = liquid nitrogen temperature, K
s
ization established in the Decision on Principles for the
X = relative pressure, P /P
2 0
Development of International Standards, Guides and Recom-
3
V = volume of manifold, cm
d
mendations issued by the World Trade Organization Technical
3
V = extra volume bulb, cm
x
Barriers to Trade (TBT) Committee.
3
V = dead-space volume, cm
s
W = mass of sample, g
2. Referenced Documents
s
W = tare mass of sample tube, g
3
1
2.1 ASTM Standards:
W = sample+tare mass of tube, g
2
D3766Terminology Relating to Catalysts and Catalysis 3
V = volume of nitrogen in the dead-space, cm
ds
E177Practice for Use of the Terms Precision and Bias in
V = see 10.4.4
1
ASTM Test Methods
V = see 10.4.6
2
E456Terminology Relating to Quality and Statistics
V = see 10.4.7
t
E691Practice for Conducting an Interlaboratory Study to
V = see 10.4.9
a
Determine the Precision of a Test Method V = see 10.8
m
T = initial extra-volume bulb temperature, K
1x
3. Terminology
T '(i ) = initial extra-volume bulb temperature, °C
1 x
3.1 Consult Terminology D3766 for definitions of other T = extra-volume bulb temperature after equilibrium,
2 x
terms used. K
T '(i ) = extra-volume bulb temperature after equilibrium,
2 x
1
°C
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.
4. Summary of Test Method
Current edition approved Oct. 1, 2020. Published November 2020. Originally
approved in 1978. Last previous edition approved in 2015 as D3663–03(2015).
4.1 The surface area of a catalyst or catalyst carrier is
DOI: 10.1520/D3663-20.
2 determined by measuring the amount of nitrogen gas adsorbed
Brunauer, Emmett, Teller, Journal of American Chemical Society, JACS, No.
60, 1938, p. 309.
at various low-pressure levels by the catalyst sample. Pressure
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
differentials caused by introducing the catalyst surface area to
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
a fixed volume of nitrogen in the test apparatus are measured
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. and used to calculate BET surface area.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D3663 − 20
4
5. Apparatus 5.6.1 It is preferred that the manifold be thermostated at a
particulartemperature,afewdegreesaboveambient,toobviate
5.1 Aschematicdiagramofasuitableapparatusisshownin
the necessity of recording this temperature at each reading.
Fig. 1. It may be const
...

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: D3663 − 03 (Reapproved 2015) D3663 − 20
Standard Test Method for
1
Surface Area of Catalysts and Catalyst Carriers
This standard is issued under the fixed designation D3663; 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 determination of surface areas of catalyst and catalyst carriers that have Type II or IV nitrogen
2
adsorption isotherms, and at least 1 m /g of area. A volumetric measuring system is used to obtain at least four data points which
2
fit on the linear BET equation line.
1.2 Units—The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information
only.after SI units are provided for information only and are not considered standard.
1.3 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 establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 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
3
2.1 ASTM Standards:
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 Consult Terminology D3766 for definitions of other terms used.
3.2 Definitions:
3.2.1 surface area of a catalyst—catalyst, n—the total probe accessible surface of the catalyst. Itcatalyst; it is expressed in square
metres per gram.
3.3 Symbols:
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 April 1, 2015Oct. 1, 2020. Published June 2015November 2020. Originally approved in 1978. Last previous edition approved in 20082015 as
D3663 – 03 (2008).(2015). DOI: 10.1520/D3663-03R15.10.1520/D3663-20.
2
Brunauer, Emmett, Teller, Journal of American Chemical Society, JACS, No. 60, 1938, p. 309.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 ----------------------
D3663 − 20
P = initial helium pressure, torr
H
1
P = helium pressure after equilibration, torr
H
2
T = temperature of manifold at initial helium pressure, °C
H
1
T = temperature of manifold after equilibration, °C
H
2
P = initial N pressure, torr
1 2
T = manifold temperature at initial N pressure, K
1 2
T ' = manifold temperature at initial N pressure, °C
1 2
P = pressure after equilibration, torr
2
P = liquid nitrogen vapor pressure, torr
0
T = liquid nitrogen temperature, K
s
X = relative pressure, P /P
2 0
3
V = volume of manifold, cm
d
3
V = extra volume bulb, cm
x
3
V = dead-space volume, cm
s
W = mass of sample, g
s
W = tare mass of sample tube, g
1
W = sample + tare mass of tube, g
2
3
V = volume of nitrogen in the dead-space, cm
ds
V = see 10.4.4
1
V = see 10.4.6
2
V = see 10.4.7
t
V = see 10.4.9
a
V = see 10.8
m
T = initial extra-volume bulb temperature, K
1x
T '(i ) = initial extra-volume bulb temperature, °C
1 x
T = extra-volume bulb temperature after equilibrium, K
2 x
T '(i ) = extra-volume bulb temperature after equilibrium, °C
2 x
4. Summary of Test Method
4.1 The surface area of a catalyst or catalyst carrier is determined by measuring the volumeamount of nitrogen gas adsorbed at
various low-pressure levels by the catalyst sample. Pressure differentials caused by introducing the catalyst surface area to a fixed
volume of nitrogen in the test apparatus are measured an
...