ASTM D4780-12
(Test Method)Standard Test Method for Determination of Low Surface Area of Catalysts and Catalyst Carriers by Multipoint Krypton Adsorption
Standard Test Method for Determination of Low Surface Area of Catalysts and Catalyst Carriers by Multipoint Krypton Adsorption
SIGNIFICANCE AND USE
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 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.
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 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.
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Designation: D4780 − 12
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.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 = helium pressure after equilibration, torr.
H2
T = temperature of manifold at initial helium
1.1 Thistestmethodcoversthedeterminationofthespecific H1
pressure, °C.
surface area of catalysts and catalyst carriers in the range from
2
T = temperature of manifold after equilibration, °C.
H2
0.05 to 10 m /g. A volumetric measuring system is used to
P = initial Kr pressure, torr.
1
obtainatleastthreedatapointswhichfallwithinthelinearBET
T' = manifold temperature at initial Kr pressure, K.
1
region.
T = manifold temperature at initial Kr pressure, °C.
1
1.2 The values stated in SI units are to be regarded as
P = Kr pressure after equilibration, torr.
2
standard. No other units of measurement are included in this
T' = manifold temperature at P,K.
2 2
T = manifold temperature at P , °C.
standard.
2 2
P = liquid nitrogen vapor pressure, torr.
o,N
1.3 This standard does not purport to address all of the
P = calculated krypton vapor pressure, torr.
o,krypton
safety concerns, if any, associated with its use. It is the
T' = liquid nitrogen temperature, K.
s
responsibility of the user of this standard to establish appro-
X = relative pressure, P /P .
2 o,krypton
priate safety and health practices and determine the applica- 3
V = volume of manifold, cm .
d
3
bility of regulatory limitations prior to use.
V = the apparent dead-space volume, cm .
s
W = weight of sample, g.
s
2. Referenced Documents
W = tare weight of sample tube, g.
1
2
2.1 ASTM Standards:
W = weight of sample plus tare weight of tube, g.
2
3
D3663Test Method for Surface Area of Catalysts and V = volume of krypton in the dead space, cm.
ds
V = See 11.3.5.
Catalyst Carriers
1
V = See 11.3.6.
D3766Terminology Relating to Catalysts and Catalysis 2
V = See 11.3.7.
E177Practice for Use of the Terms Precision and Bias in t
V = See 11.3.9.
ASTM Test Methods a
V = See 11.6.
m
E456Terminology Relating to Quality and Statistics
E691Practice for Conducting an Interlaboratory Study to
4. Summary of Test Method
Determine the Precision of a Test Method
4.1 A catalyst or catalyst carrier sample is degassed by
3. Terminology
heating in vacuum to remove absorbed vapors from the
surface. The quantity of krypton adsorbed at various low
3.1 Definitions—Consult Terminology D3766.
pressure levels is determined by measuring pressure differen-
3.2 Symbols:
tials after introduction of a fixed volume of krypton to the
sampleatliquidnitrogentemperature.Thespecificsurfacearea
is then calculated from the sample weight and adsorption data
P = initial helium pressure, torr.
H1
using the BET equation.
5. Significance and Use
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-
5.1 This test method has been found useful for the determi-
Chemical Properties.
nation of the specific surface area of catalysts and catalyst
CurrenteditionapprovedMay1,2012.PublishedJuly2012.Originallyapproved
2
carriers in the range from 0.05 to 10 m /g for materials
in 1988. Last previous edition approved in 2007 as D4780–95(2007). DOI:
10.1520/D4780-12.
specification, manufacturing control, and research and devel-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
opment in the evaluation of catalysts. The determination of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
surface area of catalysts and catalyst carriers above 10 m /g is
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. addressed in Test Method D3663.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4780 − 12
6. Apparatus and has greater precision, or a resistance thermometer from
which P values may be derived.
o,N
6.1 AschematicdiagramoftheapparatusisshowninFig.1.
It may be constructed of glass or of metal and may operate
7. Reagents
manually or automatically. It has the following features:
7.1 Purity of Reagents—Reagent grade chemicals shall be
6.1.1 Vacuum System, capable of attaining pressures below
-4
used in all tests. Unless otherwise indicated, it is intended that
10 torr (1 torr=133.3 Pa). This will include a vacuum gage
all reagents shall conform to the spe
...
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:D4780–95 (Reapproved 2007) Designation:D4780–12
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.Anumber 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 Thistestmethodcoversthedeterminationofthespecificsurfaceareaofcatalystsandcatalystcarriersintherangefrom0.05
2
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
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:
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
T8 = manifold temperature at initial Kr pressure, K.
1
T = manifold temperature at initial Kr pressure, °C.
1
P = Kr pressure after equilibration, torr.
2
T8 = 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
T8 = 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
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 Sept.May 1, 2007.2012. Published October 2007.July 2012. Originally approved in 1988. Last previous edition approved in 20012007 as
D4780–95(20017). DOI: 10.1520/D4780-95R07.10.1520/D4780-12.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.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 ----------------------
D4780–12
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 11.3.6.
2
V = See 11.3.7.
t
V = See 11.3.9.
a
V = See 11.6.
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
afixedvolumeofkryptontothesampleatliquidnitrogentemperature.Thespecificsurfaceareaisthencalculatedfromthesample
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
2
in the range from 0.05 to 10 m /g for materials specification, manufacturing control, and research and development in the
2
evaluation of catalysts. The determination of surface area of catalysts and catalyst carriers above 10 m /g is addressed in Test
Method D3663.
6. Apparatus
6.1 A schematic diagram of the apparatus is shown in Fig. 1. It may be constructed of glass or of metal and may operate
manually or automatically. It has the following features:
-4
6.1.1 Vacuum System, capable of attaining
...
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