ASTM D3663-03(2015)

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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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: Historical
• Publication Date: 31-Mar-2015
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.01 - Physical-Chemical Properties

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D3663 − 03 (Reapproved 2015)
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
P = initial helium pressure, torr
1.1 This test method covers the determination of surface H
1
P = helium pressure after equilibration, torr
H
areas of catalyst and catalyst carriers that have Type II or IV
2
2
T = temperatureofmanifoldatinitialheliumpressure,
H
nitrogen adsorption isotherms, and at least 1 m /g of area. A
1
°C
volumetricmeasuringsystemisusedtoobtainatleastfourdata
2 T = temperature of manifold after equilibration, °C
H
points which fit on the linear BET equation line. 2
P = initial N pressure, torr
1 2
1.2 The values stated in SI units are to be regarded as the
T = manifold temperature at initial N pressure, K
1 2
standard. The values given in parentheses are for information
T ' = manifold temperature at initial N pressure, °C
1 2
only. P = pressure after equilibration, torr
2
P = liquid nitrogen vapor pressure, torr
0
1.3 This standard does not purport to address all of the
T = liquid nitrogen temperature, K
s
safety concerns, if any, associated with its use. It is the
X = relative pressure, P /P
2 0
responsibility of the user of this standard to establish appro-
3
V = volume of manifold, cm
d
priate safety and health practices and determine the applica- 3
V = extra volume bulb, cm
x
bility of regulatory limitations prior to use. 3
V = dead-space volume, cm
s
W = mass of sample, g
s
2. Referenced Documents
W = tare mass of sample tube, g
1
3
2.1 ASTM Standards: W = sample+tare mass of tube, g
2
3
V = volume of nitrogen in the dead-space, cm
D3766Terminology Relating to Catalysts and Catalysis
ds
V = see 10.4.4
E177Practice for Use of the Terms Precision and Bias in
1
V = see 10.4.6
ASTM Test Methods 2
V = see 10.4.7
E456Terminology Relating to Quality and Statistics t
V = see 10.4.9
a
E691Practice for Conducting an Interlaboratory Study to
V = see 10.8
m
Determine the Precision of a Test Method
T = initial extra-volume bulb temperature, K
1x
T '(i ) = initial extra-volume bulb temperature, °C
1 x
3. Terminology
T = extra-volume bulb temperature after equilibrium,
2 x
3.1 Consult Terminology D3766 for definitions of other
K
terms used.
T '(i ) = extra-volume bulb temperature after equilibrium,
2 x
°C
3.2 Definitions:
3.2.1 surface area of a catalyst—the total surface of the
4. Summary of Test Method
catalyst. It is expressed in square metres per gram.
4.1 The surface area of a catalyst or catalyst carrier is
3.3 Symbols:
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
1
This test method is under the jurisdiction of ASTM Committee D32 on
a fixed volume of nitrogen in the test apparatus are measured
Catalysts and is the direct responsibility of Subcommittee D32.01 on Physical-
Chemical Properties.
and used to calculate BET surface area.
Current edition approved April 1, 2015. Published June 2015. Originally
4
approved in 1978. Last previous edition approved in 2008 as D3663–03 (2008).
5. Apparatus
DOI: 10.1520/D3663-03R15.
2
5.1 AschematicdiagramoftheapparatusisshowninFig.1.
Brunauer, Emmett, Teller, Journal of American Chemical Society,JACS, No.
60, 1938, p. 309.
It may be constructed of glass or of metal. It has the following
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
features:
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
4
the ASTM website. Automated equipment is commercially available.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D3663 − 03 (2015)
FIG. 1 Schematic Diagram of Surface Area Apparatus
5.1.1 Distribution Manifold, having a volume between 20 commercial instrument as a pressure saturation tube, from
3 3
and 35 cm,(V ), known to the nearest 0.05 cm . This volume which P values may be derived.
d 0
is defined as the volume between the stopcocks or valves and
6. Reagents
includes the pressure gauge.
5.1.2 Vacuum System, capable of attaining pressures below
6.1 Purity of Reagents—Reagent grade chemicals shall be
−4
10 torr(1torr=133.3Pa).Thiswillincludeavacuumgauge
used in all tests. Unless otherwise indicated, it is intended that
(not shown in Fig.
...

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 2008) D3663 − 03 (Reapproved 2015)
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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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
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—the total surface of the catalyst. It is expressed in square metres per gram.
3.3 Symbols:
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
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, 2008April 1, 2015. Published April 2008June 2015. Originally approved in 1978. Last previous edition approved in 20032008 as
D3663D3663 – 03 (2008).–03. DOI: 10.1520/D3663-03R08.10.1520/D3663-03R15.
2
Brunauer, Emmett, Teller, Journal of American Chemical Society, JACS, No. 60, 1938, p. 309.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 − 03 (2015)
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 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.
4
5. Apparatus
5.1 A schematic diagram of the apparatus is shown in Fig. 1. It may be constructed of glass or of metal. It has the following
features:
3 3
5.1.1 Distribution Manifold, having a volume between 20 and 35 cm , (V ), known to the nearest 0.05 cm . This volume is
d
defined as the volume between the stopcocks or valves
...