ASTM D3663-03

Standard Test Method for Surface Area of Catalysts and Catalyst Carriers

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 BET 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: 30-Sep-2003
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.01 - Physical-Chemical Properties

Relations

• Replaces: ASTM D3663-99 - Standard Test Method for Surface Area of Catalysts and Catalyst Carriers
• Effective Date: 01-Oct-2003
• Replaced By: ASTM D3663-03(2008) - Standard Test Method for Surface Area of Catalysts and Catalyst Carriers
• Effective Date: 01-Apr-2008
• Referred By: ASTM D4222-20 - Standard Test Method for Determination of Nitrogen Adsorption and Desorption Isotherms of Catalysts and Catalyst Carriers by Static Volumetric Measurements
• Effective Date: 01-Oct-2003
• Referred By: 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: 01-Oct-2003
• Referred By: ASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements
• Effective Date: 01-Oct-2003
• Referred By: ASTM D4567-19 - Standard Test Method for Single-Point Determination of Specific Surface Area of Catalysts and Catalyst Carriers Using Nitrogen Adsorption by Continuous Flow Method
• Effective Date: 01-Oct-2003
• Referred By: ASTM D4365-19 - Standard Test Method for Determining Micropore Volume and Zeolite Area of a Catalyst
• Effective Date: 01-Oct-2003
• Referred By: ASTM D4463/D4463M-19 - Standard Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
• Effective Date: 01-Oct-2003
• Referred By: ASTM D1319-20a - Standard Test Method for Hydrocarbon Types in Liquid Petroleum Products by Fluorescent Indicator Adsorption
• Effective Date: 01-Oct-2003

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
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope
P = helium pressure after equilibration, torr
H
2
T = temperature of manifold at initial helium pres-
1.1 This test method covers the determination of surface H
1
sure, °C
areas of catalyst and catalyst carriers that have Type II or IV
2
T = temperature of manifold after equilibration, °C
nitrogen adsorption isotherms, and at least 1 m /g of area. A H
2
P = initial N pressure, torr
1 2
volumetricmeasuringsystemisusedtoobtainatleastfourdata
T = manifold temperature at initial N pressure, K
2
1 2
points which fit on the linear BET line.
T 8 = manifold temperature at initial N pressure, °C
1 2
1.2 The values stated in SI units are to be regarded as the
P = pressure after equilibration, torr
2
standard. The values given in parentheses are for information
P = liquid nitrogen vapor pressure, torr
0
only.
T = liquid nitrogen temperature, K
s
1.3 This standard does not purport to address all of the
X = relative pressure, P /P
2 0
3
safety concerns, if any, associated with its use. It is the
V = volume of manifold, cm
d
3
responsibility of the user of this standard to establish appro-
V = extra volume bulb, cm
x
3
priate safety and health practices and determine the applica-
V = dead-space volume, cm
s
bility of regulatory limitations prior to use.
W = mass of sample, g
s
W = tare mass of sample tube, g
1
2. Referenced Documents
W = sample+tare mass of tube, g
2
3
3
V = volume of nitrogen in the dead-space, cm
2.1 ASTM Standards:
ds
V = see 10.4.4
D3766 Terminology Relating to Catalysts and Catalysis 1
V = see 10.4.6
E177 Practice for Use of the Terms Precisions and Bias in 2
V = see 10.4.7
t
ASTM Test Methods
V = see 10.4.9
a
E456 Terminology Relating to Quality and Statistics
V = see 10.8
m
E691 Practice for Conducting an Interlaboratory Study to
T = initial extra-volume bulb temperature, K
1x
Determine the Precision of a Test Method
T 8(i) = initial extra-volume bulb temperature, °C
1x
T = extra-volume bulb temperature after equilibrium,
2x
3. Terminology
K
3.1 Consult Terminology D3766 for definitions of other
T 8(i) = extra-volume bulb temperature after equilibrium,
2x
terms used.
°C
3.2 Definition:
3.2.1 surface area of a catalyst—the total surface of the
4. Summary of 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
P = initial helium pressure, torr
H
1
a fixed volume of nitrogen in the test apparatus are measured
and used to calculate BET surface area.
1
4
This test method is under the jurisdiction of ASTM Committee D32 on
5. Apparatus
Catalysts and is the direct responsibility of Subcommittee D32.01 on Physical-
5.1 AschematicdiagramoftheapparatusisshowninFig.1.
Chemical Properties.
Current edition approved Oct. 1, 2003. Published October 2003. Originally
It may be constructed of glass or of metal. It has the following
approved in 1978. Last previous edition approved in 1999 as D3663–99.
features:
2
Brunauer, Emmett, Teller, Journal of American Chemical Society, JACS, No.
5.1.1 Distribution Manifold, having a volume between 20
60, 1938, p. 309.
3 3
3
and 35 cm,(V ), known to the nearest 0.05 cm . This volume
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
d
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.
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D3663–03
FIG. 1 Schematic Diagram of Surface Area Apparatus
is defined as the volume between the stopcocks or valves and all reagents shall conform to the specifications of the Commit-
includes the pressure gage. tee onAnalytical Reagents of theAmerican Chemical Society,
6
5.1.2 Vacuum System, capable of attaining pressures below where such specifications are available. Other grades may be
−4
10 torr (1 torr=133.3 Pa). This will include a vacuum gage used, provided it is first ascertained that the reagent is of
(not shown in Fig. 1). Access to the distribution manifold
...