ASTM D4780-23

Standard Test Method for Determination of Low Surface Area of Catalysts and Catalyst Carriers by Multipoint Krypton Adsorption

SIGNIFICANCE AND USE
5.1 This test method has been found useful for the determination of the specific surface area of catalysts and catalyst carriers in the range from 0.05 m2/g to 10 m2/g for materials specification, manufacturing control, and research and development in the evaluation of catalysts. The determination of surface area of catalysts and catalyst carriers above 10 m2/g is addressed in Test Method D3663 – Surface Area of Catalyst and Catalyst Carriers – and is appropriate for most samples with specific surface areas above 1 m2/g.
SCOPE
1.1 This test method covers the determination of the specific surface area of catalysts and catalyst carriers in the range from 0.05 m2/g to 10 m2/g. A volumetric measuring system is used to obtain at least three data points which fall within the linear BET region.  
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 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Published
• Publication Date: 14-Oct-2023
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.01 - Physical-Chemical Properties

Relations

• Replaces: ASTM D4780-12(2017)e1 - Standard Test Method for Determination of Low Surface Area of Catalysts and Catalyst Carriers by Multipoint Krypton Adsorption
• Effective Date: 15-Oct-2023

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: D4780 − 23
Standard Test Method for
Determination of Low Surface Area of Catalysts and
1
Catalyst Carriers by Multipoint Krypton Adsorption
This standard is issued under the fixed designation D4780; 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
P = initial helium pressure, torr.
1.1 This test method covers the determination of the specific
H1
P = helium pressure after equilibration, torr.
H2
surface area of catalysts and catalyst carriers in the range from
2 2
T = temperature of manifold at initial helium
H1
0.05 m /g to 10 m /g. A volumetric measuring system is used
pressure, °C.
to obtain at least three data points which fall within the linear
T = temperature of manifold after equilibration, °C.
H2
BET region.
P = initial Kr pressure, torr.
1
1.2 The values stated in SI units are to be regarded as
T' = manifold temperature at initial Kr pressure, K.
1
standard. No other units of measurement are included in this
T = manifold temperature at initial Kr pressure, °C.
1
standard.
P = Kr pressure after equilibration, torr.
2
T' = manifold temperature at P , K.
1.3 This standard does not purport to address all of the 2 2
T = manifold temperature at P , °C.
2 2
safety concerns, if any, associated with its use. It is the
P = liquid nitrogen vapor pressure, torr.
o,N
responsibility of the user of this standard to establish appro-
P = calculated krypton vapor pressure, torr.
o,krypton
priate safety and health practices and determine the applica-
T' = liquid nitrogen temperature, K.
s
bility of regulatory limitations prior to use.
X = relative pressure, P /P .
2 o,krypton
3
V = volume of manifold, cm .
2. Referenced Documents d
3
V = the apparent dead-space volume, cm .
2
s
2.1 ASTM Standards:
W = weight of sample, g.
s
D3663 Test Method for Surface Area of Catalysts and
W = tare weight of sample tube, g.
1
Catalyst Carriers
W = weight of sample plus tare weight of tube, g.
2
3
D3766 Terminology Relating to Catalysts and Catalysis
V = volume of krypton in the dead space, cm.
ds
E105 Guide for Probability Sampling of Materials
V = See 12.3.5.
1
E122 Practice for Calculating Sample Size to Estimate, With
V = See 12.3.6.
2
Specified Precision, the Average for a Characteristic of a V = See 12.3.7.
t
Lot or Process V = See 12.3.9.
a
V = See 12.6.
E177 Practice for Use of the Terms Precision and Bias in
m
ASTM Test Methods
4. Summary of Test Method
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to
4.1 A catalyst or catalyst carrier sample is degassed by
Determine the Precision of a Test Method
heating in vacuum to remove absorbed vapors from the
surface. The quantity of krypton adsorbed at various low
3. Terminology
pressure levels is determined by measuring pressure differen-
3.1 Definitions—Consult Terminology D3766.
tials after introduction of a fixed volume of krypton to the
sample at liquid nitrogen temperature. The specific surface area
3.2 Symbols:
is then calculated from the sample weight and adsorption data
1
using the BET equation.
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.
5. Significance and Use
Current edition approved Oct. 15, 2023. Published November 2023. Originally
ɛ1
5.1 This test method has been found useful for the determi-
approved in 1988. Last previous edition approved in 2017 as D4780 – 12 (2017) ).
DOI: 10.1520/D4780-23.
nation of the specific surface area of catalysts and catalyst
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 2 2
carriers in the range from 0.05 m /g to 10 m /g for materials
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
specification, manufacturing control, and research and devel-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. opment in the evaluation of catalysts. The determination of
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4780 − 23
2 −7
surface area of catalysts and catalyst carriers above 10 m /g is 6.1.10 Laboratory Balance with 0.1 mg (10 kg) sensitiv-
addressed in Test Method D3663 – Surface Area of Catalyst ity.
and Catalyst Carriers – and is appropriate for most samples 6.1.
...

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.
´1
Designation: D4780 − 12 (Reapproved 2017) D4780 − 23
Standard Test Method for
Determination of Low Surface Area of Catalysts and
1
Catalyst Carriers by Multipoint Krypton Adsorption
This standard is issued under the fixed designation D4780; 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
ε NOTE—Subsesction 8.1 was corrected editorially in February 2017.
1. Scope
1.1 This test method covers the determination of the specific surface area of catalysts and catalyst carriers in the range from
2 2
0.050.05 m to 10 m/g to 10 m /g. A volumetric measuring system is used to obtain at least three data points which fall within the
linear BET region.
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 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 and health practices and determine the applicability of regulatory
limitations prior to use.
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
E105 Guide for Probability Sampling of Materials
E122 Practice for Calculating Sample Size to Estimate, With Specified Precision, the Average for a Characteristic of a Lot or
Process
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—Consult Terminology D3766.
3.2 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 Feb. 1, 2017Oct. 15, 2023. Published February 2017November 2023. Originally approved in 1988. Last previous edition approved in 20122017
ɛ1
as D4780D4780 – 12 (2017) –12). DOI: 10.1520/D4780-12R17.). DOI: 10.1520/D4780-23.
2
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 ----------------------
D4780 − 23
P = initial helium pressure, torr.
H1
P = helium pressure after equilibration, torr.
H2
T = temperature of manifold at initial helium pressure, °C.
H1
T = temperature of manifold after equilibration, °C.
H2
P = initial Kr pressure, torr.
1
T' = manifold temperature at initial Kr pressure, K.
1
T = manifold temperature at initial Kr pressure, °C.
1
P = Kr pressure after equilibration, torr.
2
T' = manifold temperature at P , K.
2 2
T = manifold temperature at P , °C.
2 2
P = liquid nitrogen vapor pressure, torr.
o,N
P = calculated krypton vapor pressure, torr.
o,krypton
T' = liquid nitrogen temperature, K.
s
X = relative pressure, P /P .
2 o,krypton
3
V = volume of manifold, cm .
d
3
V = the apparent dead-space volume, cm .
s
W = weight of sample, g.
s
W = tare weight of sample tube, g.
1
W = weight of sample plus tare weight of tube, g.
2
3
V = volume of krypton in the dead space, cm.
ds
V = See 11.3.5.
1
V = See 12.3.5.
1
V = See 11.3.6.
2
V = See 12.3.6.
2
V = See 11.3.7.
t
V = See 12.3.7.
t
V = See 11.3.9.
a
V = See 12.3.9.
a
V = See 11.6.
m
V = See 12.6.
m
4. Summary of Test Method
4.1 A catalyst or catalyst carrier sample is degassed by heating in vacuum to remove absorbed vapors from the surface. The
quantity of krypton adsorbed at various low pressure levels is determined by measuring pressure differentials after introduction of
a fixed volume of krypton to the sample at liquid nitrogen temperature. The specific surface area is then calculated from the sample
weight and adsorption data using the BET equation.
5. Significance and Use
5.1 This test method has been found useful for the determination of the specific surface area of catalysts and catalyst carriers in
2 2
the range from 0.050.05 m to 10 m/g to 10 m /g
...