ASTM D4222-03(2008)

Standard Test Method for Determination of Nitrogen Adsorption and Desorption Isotherms of Catalysts and Catalyst Carriers by Static Volumetric Measurements

SIGNIFICANCE AND USE
The test method has two main functions: first, it provides data useful for establishing the pore size distribution of catalyst materials, which in turn may influence their performance; and second, it serves as a laboratory test which may be used to study porosity changes that may occur during the manufacture and evaluation of catalysts.
SCOPE
1.1 This test method covers the determination of nitrogen adsorption and desorption isotherms of catalysts and catalyst carriers at the boiling point of liquid nitrogen. A static volumetric measuring system is used to obtain sufficient equilibrium adsorption points on each branch of the isotherm to adequately define the adsorption and desorption branches of the isotherm. Thirty points evenly spread over the isotherm is considered to be the minimum number of points that will adequately define the isotherm.
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-2008
• ICS: 17.060 - Measurement of volume, mass, density, viscosity
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.01 - Physical-Chemical Properties

Relations

• Replaces: ASTM D4222-03 - Standard Test Method for Determination of Nitrogen Adsorption and Desorption Isotherms of Catalysts By Static Volumetric Measurements
• Effective Date: 01-Apr-2008
• Referred By: ASTM D4641-17 - Standard Practice for Calculation of Pore Size Distributions of Catalysts and Catalyst Carriers from Nitrogen Desorption Isotherms
• Effective Date: 01-Apr-2008
• Referred By: ASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements
• Effective Date: 01-Apr-2008

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4222 − 03(Reapproved 2008)
Standard Test Method for
Determination of Nitrogen Adsorption and Desorption
Isotherms of Catalysts and Catalyst Carriers by Static
1
Volumetric Measurements
This standard is issued under the fixed designation D4222; 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. Terminology
1.1 This test method covers the determination of nitrogen 3.1 Definitions—See Terminology D3766.
adsorption and desorption isotherms of catalysts and catalyst
3.2 Symbols:
2
carriers at the boiling point of liquid nitrogen. A static
volumetric measuring system is used to obtain sufficient
equilibriumadsorptionpointsoneachbranchoftheisothermto
PH = initial helium pressure, torr.
1
adequately define the adsorption and desorption branches of PH = helium pressure after equilibration, torr.
2
TH = temperature of manifold at initial helium pressure,
the isotherm. Thirty points evenly spread over the isotherm is
1
°C.
considered to be the minimum number of points that will
TH = temperature of manifold after equilibration, °C.
adequately define the isotherm.
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
T = manifold temperature after equilibrrium, K.
1.3 This standard does not purport to address all of the
2
T' = manifold temperature after equilibrium, °C.
safety concerns, if any, associated with its use. It is the 2
P = initial N pressure during desorption, torr.
responsibility of the user of this standard to establish appro- 3 2
T = manifold temperature at initial N pressure, K.
3 2
priate safety and health practices and determine the applica-
T' = manifold temperature at initial N pressure, °C.
3 2
bility of regulatory limitations prior to use.
P = pressure after equilibration during desorption, torr.
4
T = manifold temperature after equilibration, K.
4
2. Referenced Documents
T' = manifold temperature after equilibration, °C.
4
3
2.1 ASTM Standards: P = liquid nitrogen vapor pressure, torr.
0
D3663Test Method for Surface Area of Catalysts and T = liquid nitrogen temperature, K.
s
X = relative pressure, P /P .
Catalyst Carriers
2(4) 0
3
V = volume of manifold, cm .
D3766Terminology Relating to Catalysts and Catalysis d
3
V = the dead-space volume factor, cm (STP)/torr.
s
E177Practice for Use of the Terms Precision and Bias in
W = mass of sample, g.
s
ASTM Test Methods
W = tare of sample tube, g.
1
E456Terminology Relating to Quality and Statistics
W' = sample mass + tare of tube after degassing, g.
2
E691Practice for Conducting an Interlaboratory Study to
W = sample mass + tare of tube after adsorption, g.
2
Determine the Precision of a Test Method 3
V = volume of nitrogen in the dead-space, cm (STP).
ds
V = see 12.4.3.
1
V = see 12.4.4.
2
1
V = see 12.4.5.
ThistestisunderthejurisdictionofASTMCommitteeD32onCatalystsandis
t
the direct responsibility of Subcommittee D32.01 on Physical-Chemical Properties. V = see 12.4.7.
ad
Current edition approved April 1, 2008. Published April 2008. Originally
V = see 12.5.
de
approved in 1983. Last previous edition approved in 2003 as D4222–03. DOI:
10.1520/D4222-03R08.
4. Summary of Test Method
2
Adamson,A. W., Physical Chemistry of Surfaces, 3rd ed., John Wiley & Sons,
New York, NY, 1976, p. 532.
4.1 Thesampleisheatedandevacuatedtoremoveadsorbed
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
vapors from the surface.The nitrogen adsorption branch of the
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
isotherm is determined by evacuating the sample, cooling the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sample to the boiling point of liquid nitrogen (;77.3 K), and
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4222 − 03 (2008)
6.1.3 Pressure Sensing Devices or Pressure Transducers,
capable of measurements with a sensitivity of at least 0.1 torr,
in the range from 0 to 1000 torr (1 torr = 133.3 Pa).
6.1.4 Value (H), from the helium supply to the distribution
manifold.
6.1.5 Valve (N), from the nitrogen supply to the distribution
manifold.
6.1.6 The connection between the sample tube and the S
valve can be a standard-taper glass joint, a glass-to-glass
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D4222–98 Designation: D 4222 – 03 (Reapproved 2008)
Standard Test Method for
Determination of Nitrogen Adsorption and Desorption
Isotherms of Catalysts Byand Catalyst Carriers by Static
1
Volumetric Measurements
This standard is issued under the fixed designation D4222; 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
1.1 This test method covers the determination of nitrogen adsorption and desorption isotherms of catalysts and catalyst carriers
2
at the boiling point of liquid nitrogen. A static volumetric measuring system is used to obtain sufficient equilibrium adsorption
points on each branch of the isotherm to adequately define the adsorption and desorption branches of the isotherm. Thirty points
evenly spread over the isotherm is considered to be the minimum number of points that will adequately define the isotherm.
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:
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— Consult Terminology D 3766— See Terminology D3766.
3.2 Symbols:
PH = initial helium pressure, torr.
1
PH = helium pressure after equilibration, torr.
2
TH = temperature of manifold at initial helium pressure, °C.
1
TH = temperature of manifold after equilibration, °C.
2
P = initial N pressure, torr.
1 2
T = manifold temperature at initial N pressure, K.
1 2
T8 = manifold temperature at initial N pressure, °C.
1 2
P = pressure after equilibration, torr.
2
T = manifold temperature after equilibrrium, K.
2
T8 = manifold temperature after equilibrium, °C.
2
P = initial N pressure during desorption, torr.
3 2
T = manifold temperature at initial N pressure, K.
3 2
T8 = manifold temperature at initial N pressure, °C.
3 2
1
This test is under the jurisdiction of ASTM Committee D-32 on Catalysts and is the direct responsibility of Subcommittee D32.01 on Physical-Chemical Properties.
Current edition approved March 10, 1998. Published November 1998. Originally published as D 4222 - 83. Last previous edition D 4222 - 91.
1
This test 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, 2008. Published April 2008. Originally approved in 1983. Last previous edition approved in 2003 as D4222–03.
2
Annual Book of ASTM Standards, Vol 05.03.
2
Adamson, A. W., Physical Chemistry of Surfaces, 3rd ed., John Wiley & Sons, New York, NY, 1976, p. 532.
3
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,[e-mail] Annual Book of ASTM Standards
, Vol 14.02.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 ----------------------
D 4222 – 03 (2008)
P = pressure after equilibration during desorption, torr.
4
T = manifold temperature after equilibration, K.
4
T8 = manifold temperature after equilibration, °C.
4
P = liquid nitrogen vapor pressure, torr.
0
T = liquid nitrogen temperature, K.
s
X = relative pressure, P 2(4)/P .
2(4) 0
3
V = volume of manifold, cm .
d
3
V = the dead-space volume factor, cm (STP)/torr.
s
W = weightmass of sample, g.
s
W = tare weight of sample tube, g.
1
W8 = sample mass + tare weight of tube after degassing, g.
2
W = sample mass + tare weight of tube after adsorption, g.
2
3
V = volume of nitrogen in the dead-space, cm (STP).
ds
V = see 12.4.5see 12.4.3.
1
V = see 12.4.7see 12.4.4.
2
V = see 12.4.8. see 12.4
...