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: D3663 − 20

Standard Test Method for

Surface Area of Catalysts and Catalyst Carriers1
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 3.2 Definitions:

1.1 This test method covers the determination of surface 3.2.1 surface area of a catalyst, n—the total probe acces-
areas of catalyst and catalyst carriers that have Type II or IV sible surface of the catalyst; it is expressed in square metres per
nitrogen adsorption isotherms, and at least 1 m2/g of area. A gram.
volumetric measuring system is used to obtain at least four data 3.3 Symbols:
points which fit on the linear BET2 equation line.
1.2 Units—The values stated in SI units are to be regarded
as standard. The values given in parentheses after SI units are P H1 = initial helium pressure, torr
PH2 = helium pressure after equilibration, torr
provided for information only and are not considered standard.
T H1 = temperature of manifold at initial helium pressure,
1.3 This standard does not purport to address all of the °C
safety concerns, if any, associated with its use. It is the TH2 = temperature of manifold after equilibration, °C
responsibility of the user of this standard to establish appro- P1 = initial N2 pressure, torr
priate safety, health, and environmental practices and deter- T1 = manifold temperature at initial N2 pressure, K
mine the applicability of regulatory limitations prior to use. T 1' = manifold temperature at initial N2 pressure, °C
1.4 This international standard was developed in accor- P2 = pressure after equilibration, torr
dance with internationally recognized principles on standard- P0 = liquid nitrogen vapor pressure, torr
ization established in the Decision on Principles for the Ts = liquid nitrogen temperature, K
Development of International Standards, Guides and Recom- X = relative pressure, P2/P0
mendations issued by the World Trade Organization Technical Vd = volume of manifold, cm3
Barriers to Trade (TBT) Committee. Vx = extra volume bulb, cm3
Vs = dead-space volume, cm3
2. Referenced Documents Ws = mass of sample, g
W1 = tare mass of sample tube, g
2.1 ASTM Standards:3 W2 = sample + tare mass of tube, g
D3766 Terminology Relating to Catalysts and Catalysis Vds = volume of nitrogen in the dead-space, cm3
E177 Practice for Use of the Terms Precision and Bias in V1 = see 10.4.4
ASTM Test Methods V2 = see 10.4.6
E456 Terminology Relating to Quality and Statistics Vt = see 10.4.7
E691 Practice for Conducting an Interlaboratory Study to Va = see 10.4.9
Determine the Precision of a Test Method Vm = see 10.8
T1x = initial extra-volume bulb temperature, K
3. Terminology T1 x'(i ) = initial extra-volume bulb temperature, °C
3.1 Consult Terminology D3766 for definitions of other T2 x = extra-volume bulb temperature after equilibrium,
terms used. K
T2 x'(i ) = extra-volume bulb temperature after equilibrium,
1
This test method is under the jurisdiction of ASTM Committee D32 on °C
Catalysts and is the direct responsibility of Subcommittee D32.01 on Physical-
Chemical Properties.
Current edition approved Oct. 1, 2020. Published November 2020. Originally
4. Summary of Test Method
approved in 1978. Last previous edition approved in 2015 as D3663 – 03(2015).
DOI: 10.1520/D3663-20.
4.1 The surface area of a catalyst or catalyst carrier is
2
Brunauer, Emmett, Teller, Journal of American Chemical Society, JACS, No. determined by measuring the amount of nitrogen gas adsorbed
60, 1938, p. 309. at various low-pressure levels by the catalyst sample. Pressure
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or differentials caused by introducing the catalyst surface area to
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on a fixed volume of nitrogen in the test apparatus are measured
the ASTM website. and used to calculate BET surface area.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D3663 − 20
5. Apparatus4 5.6.1 It is preferred that the manifold be thermostated at a
5.1 A schematic diagram of a suitable apparatus is shown in particular temperature, a few degrees above ambient, to obviate
Fig. 1. It may be constructed of glass or of metal. Commercial the necessity of recording this temperature at each reading.
metal instruments are available. It has the following features: 5.7 Thermometer, for measuring the temperature of the
5.1.1 Distribution Manifold, having a volume between 20 liquid nitrogen bath [ Ts(i)] in kelvins. This will preferably be
and 35 cm3, (Vd), known to the nearest 0.05 cm3. This volume a nitrogen vapor-pressure thermometer, often referred to in a
is defined as the volume between the stopcocks or valves and commercial instrument as a pressure saturation tube, from
includes the pressure gauge. which P0 values may be derived.
5.1.2 Vacuum System, capable of attaining pressures below
10−4 torr (1 torr = 133.3 Pa). This can include a vacuum gauge 6. Reagents
(not shown in Fig. 1). Access to the distribution manifold is 6.1 Purity of Reagents—Reagent grade chemicals shall be
through the valve V. used in all tests. Unless otherwise indicated, it is intended that
5.1.3 Pressure-Measuring Device, that operates at constant all reagents shall conform to the specifications of the Commit-
volume and is capable of measurements to the nearest 0.1 torr, tee on Analytical Reagents of the American Chemical Society,
in the range from 0 to 1000 torr (1 torr = 133.3 Pa). where such specifications are available.6 Other grades may be
NOTE 1—See, for example, the article by Joy5 for a description of a used, provided it is first ascertained that the reagent is of
constant-volume manometer. sufficiently high purity to permit its use without lessening the
accuracy of the determination.
5.1.4 Valve (H), from the helium supply to the distribution
manifold. 6.2 Helium Gas—A cylinder of helium gas at least 99.999 %
5.1.5 Valve (N), from the nitrogen supply to the distribution pure.
manifold. 6.3 Liquid Nitrogen, of such purity that P0 is not more than
5.1.6 The connection between the sample tube and the S 20 torr above barometric pressure. A fresh daily supply is
valve can be a standard-taper glass joint, a glass-to-glass seal, recommended.
or a compression fitting.
5.1.7 Extra Volume Bulb, (Vx), should be 100 to 150 cm3, 6.4 Nitrogen Gas—A cylinder of nitrogen gas at least
known to the nearest 0.05 cm3. Vx includes the volume of the 99.999 % pure.
stopcock bore in the glass apparatus. 7. Procedure—Sample Preparation and Degassing
5.2 Sample Tubes, with volumes from 5 to 100 cm3 depend- 7.1 Select a sample tube of the desired size. A 5 cm3 sample
ing on the application. Use sample tubes recommended by the tube is preferred for samples not exceeding about 1 g, to
instrument manufacturer. If necessary, markings should be minimize the dead-space. However, a 25 cm3 sample tube may
placed on the sample tube about 30 to 50 mm below the be preferred for finely powdered catalysts, to avoid “boiling”
connectors to indicate the desired liquid nitrogen level. when degassing is started.
5.3 Heating Mantles or Small Furnaces. 7.2 Fill the sample tube with nitrogen or helium, at atmo-
5.4 Dewar Flasks. spheric pressure, after removing air by evacuation. This may be
5.5 Laboratory Balance, with 0.1 mg (10−7 kg) sensitivity. done on the surface area unit, or on a separate piece of
equipment.
5.6 Thermometer or Thermocouple, for measuring the tem-
perature of the distribution manifold [T1'(i) or T2'(i)] in degrees
6
Celsius or kelvins. Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
4
Automated equipment is commercially available. MD.
5
Joy, A. S., Vacuum, Vol 3, 1953, p. 254.

FIG. 1 Schematic Diagram of Surface Area Apparatus

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 D3663 − 20
7.3 Remove the sample tube from the system, cap, and considered equivalent to determination of dead-space by helium and can
weigh. Record the mass as W1. be used if helium is not available. Follow the recommendations of the
instrument manufacturer for these measurements.
7.4 Place the catalyst sample, whose mass is known
8.3 Place a Dewar flask of liquid nitrogen around the sample
approximately, into the sample tube. Choose the sample size to
and adjust the liquid level to a fixed point on the sample tube.
provide an estimated total sample surface area of 20 to 100 m2.
Maintain this level throughout the test.
7.5 Attach the sample tube to the apparatus. If other samples
8.4 Zero the pressure gauge.
are to be run, attach them at this time to the other ports.
8.5 Admit the helium gas into the manifold to a pressure of
7.6 Open the S valves where there are samples.
600 to 900 torr by carefully opening the H valve. Record this
7.7 It may be necessary to close the V valve system pressure as PH1, and the manifold temperature, TH1.
periodically to protect the diffusion pump fluid from exposure
8.6 Open the S valve to admit helium to the sample.
to pressures above 0.1 torr for periods of more than 30 s. Close
the valve off for 2 min. 8.7 After about 5 min of equilibration, readjust the liquid
nitrogen level, and record the pressure as PH2 , and manifold
7.8 Install a heating mantle or furnace around each sample
temperature as TH2.
and raise the temperature to about 300 °C (573 K).
8.8 Repeat 8.5 – 8.7 for each sample on the manifold.
NOTE 2—Take special precautions if the moisture content exceeds
approximately 5 % to avoid “bumping” of powdered catalyst, and to avoid 8.9 Open all S valves; then slowly open the V valve to
surface area loss by self-steaming. A stepped or pressure-controlled remove the helium gas.
heating routine is recommended under these circumstances.
NOTE 3—Not all catalysts or their supports are stable to 300 °C. This 8.10 When a pressure less than 0.01 torr has been attained,
should be noted and the appropriate temperature should be used based on close the S valve. This operation should take 5 to 10 min.
thermal properties of the material.
7.9 Continue degassing at about 300 °C (573 K) for a 9. Procedure—Nitrogen Adsorption
minimum of 3 h, at a pressure not to exceed 10−3 torr. 9.1 Close the V valve and open the EV valve if the
Overnight degassing is permissible. extra-volume bulb is to be used, when the surface area is
7.10 Remove the heating mantles, and allow the samples to known to be high.
cool. 9.2 Recheck the zero setting of the pressure gauge.
7.11 Close the EV valve, if open. 9.3 Admit nitrogen gas, and record the pressure as P1(1)
7.12 Close the S valve. (torr) and the temperature as T1'(1) (degrees Celsius) and read
the temperature of the extra-volume bulb and record it as
7.13 It is permissible to exercise the option of preliminary
T1x(1). It is desirable, but not necessary, to choose P1(1) such
degassing on an external unit. In such a case, follow the
that the first equilibrium adsorption pressure, P2(1), will be
procedures of 7.4 – 7.11 and then repeat on the surface area
about 40 torr equivalent to P2(1)/P0(1) of about 0.05. If the
unit, except that the degassing time in 7.9 should not exceed
surface area is small, it may be desirable to eliminate use of the
1 h.
extra-volume bulb by closing the EV valve.
7.14 If it is desired to weigh the sample after preliminary
degassing on an external unit, backfill with the same gas used 9.4 Open the S valve to admit nitrogen to the catalyst.
in 7.2 to above atmospheric pressure. Close the S valve. 9.5 Allow sufficient time for equilibration, readjusting the
7.15 Detach the sample tube from the apparatus, recap with liquid nitrogen level when necessary. Equilibrium shall be
the stopper used previously, and weigh. Record the mass as W2. considered as attained when the pressure change is no more
than 0.02 torr/min.
7.16 Remove the backfilled gas by evacuation to less than
10−4 torr at room temperature. 9.6 Record the equilibrium pressure as P2(1), manifold
temperature T2'(1), and the extra volume bulb temperature
8. Procedure—Dead-Space Determination T2x(1).
8.1 From this point on, each sample being tested for surface 9.7 Record the liquid nitrogen temperature [Ts(1)] or the
area must be run on an individual basis. Thus each Step (8.2 – nitrogen vapor pressure [P0(1)].
9.17) must be carried out separately for each tube in test. 9.8 Close the S valve and close the EV valve; then admit
8.2 The “dead-space” is the void volume of the charged nitrogen gas to increase the pressure by 100 to 200 torr,
sample tube, including the S valve, when the tube is immersed depending upon surface area. Record the pressure as P1(2), the
in liquid nitrogen to the proper depth (see 5.2). manifold temperature as T1'(2), and the extra-volume bulb
temperature as T1 x'(2).
NOTE 4—The dead-space may be determined after the nitrogen
adsorption, if more convenient, as long as adequate degassing precedes it. 9.9 Open the S valve to admit the new increment of nitrogen
In that case, replace the liquid nitrogen bath after Step 9.14 before to the catalyst.
proceeding with Steps 8.3 – 8.9.
NOTE 5—Some commercial equipment allows for helium-free determi- 9.10 Allow sufficient time for equilibration, readjusting the
nation of the dead-space by calibration of a blank cell and accounting for liquid nitrogen level as necessary. The criterion for equilibrium
the skeletal volume of the sample when the cell is charged. This can be is defined in 9.5.

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 D3663 − 20
9.11 Record the equilibrium pressure as P2(2), and record 10.4.3 Extra-volume bulb volume at manifold temperature
T2'(2) and T2x'(2). T1(i):
9.12 Again record Ts(2) or P0(2). V 1x 5 T 1 ~ i ! 3 V x /T 1x ~ i ! (5)
.
9.13 Repeat Steps 9.8 – 9.12 until there are at least four
points in the linear BET range. This will normally be from 10.4.4 Volume of N2 in manifold + extra volume, S valve,
P/Po = 0.04 to 0.20 or 0.25. Designate the pressures as P1(i) closed to catalyst (cm3 STP):
and P2(i), manifold temperature as T'(i ), and the extra-volume
temperatures as T1x(i) and T2x(i). (i = 3 to n, where n is total V 1 ~ i ! 5 ~ V d 1V x ! S ~~ !! D S
P1 i
T1 i
273.15
760 D (6)
number of points.)
10.4.5 Extra-Volume bulb volume at manifold temperature
9.14 Slowly open the V valve, remove the Dewar flask, and T2(i):
allow the sample flask to come to room temperature.
V 2x 5 T 2 ~ i ! 3 V x /T 2x ~ i ! (7)
9.15 When frost has disappeared from the sample tube, wipe
it dry. 10.4.6 Volume of N2 in manifold + extra volume, S valve,
open to catalyst (cm3 STP):
9.16 Backfill the sample tube with the same gas used in 7.2
to about atmospheric pressure. Close the S valve. V 2 ~ i ! 5 ~ V d 1V x ! S ~~ !! D S
P2 i
T2 i
273.15
760 D (8)
9.17 Detach the sample tube from the apparatus, recap with
the stopper used previously, and weigh. Record the mass as W2. See 5.1.1 and 5.1.7 for Vd and Vx.
10.4.7 Total inventory of nitrogen in the system (cm3 STP):
10. Calculations V t ~ i ! 5 V t ~ i 2 1 ! 1V 1 ~ i ! 2 V 2 ~ i 2 1 ! (9)
10.1 Calculate the mass of sample Ws, as follows: V t~ 0 ! 5 0
Ws 5 W2 2 W1 (1)
V 2~ 0 ! 5 0
10.2 Calculate the dead-space, Vs as follows:
10.4.8 Volume of nitrogen in the dead-space (cm3 STP):
Vs 5 S DS
T sV d
P H2
P H1
2
P H2
~ T H 11273.15! ~ T H 21273.15! D (2)
V ds~ i ! 5 S 273.15 V s 3 P 2 ~ i !
760T s DS 11
0.05 P 2 ~ i !
760 D (10)
10.3 For each point, i = 1, 2 . . . n, the following measure-
ments will have been recorded: See 10.2 for Vs.
10.3.1 For pressures P1 (i) and P2(i), see 5.1.3, 9.3, 9.6, 9.8, 10.4.8.1 The deviation from the ideal gas law of nitrogen at
9.11, and 9.13. liquid nitrogen temperature is 5 % at one atmosphere, propor-
10.3.2 For vapor pressures Po(i), or liquid nitrogen tional to pressure. Although the non-ideality constant should be
temperatures, Ts(i), see 5.7, 9.7, and 9.12. applied only to the volume of nitrogen within the section of the
sample cell that is immersed in the liquid nitrogen, the added
10.3.2.1 If P o(i) is not measured directly, the values of Ts(i)
complexity to the experimental procedure needed to determine
can be converted to P0(i) by the following equation for 76 ≤ Ts
the fraction of the volume at liquid nitrogen temperature is not
(i) ≤ 80:
justified by the increased accuracy.
P 0 ~ i ! 5 210729314269.71@ Ts~ i ! # 2 57.3616@ Ts~ i ! # 2 (3) 10.4.9 The quantity of gas adsorbed (cm3 STP/g):
10.261431@ T s ~ i ! # 3 V t ~ i ! 2 V 2 ~ i ! 2 V ds~ i !
V a~ i ! 5 (11)
Ws
10.3.3 For manifold temperatures T 1'(i) and T 2'(i), see 5.6,
9.3, 9.6, 9.8, 9.11, and 9.13. See 10.1 for W s.
10.3.4 Determine whether valve EV is open. If not, Vx = 0, 10.4.10 The BET function, when X(i) ≥ 0.04:
see 5.1.7.
10.3.5 For extra-volume bulb temperatures T1x'(i) and T2
BET ~ i ! 5 S ~~ !! D S @
X i
Va i
1
1 2 X~i!# D (12)

x'(i); see 9.3, 9.6, 9.8, and 9.11.

10.5 Construct the BET plot, by plotting X(i) as the
10.4 For each point, i = 1, 2 . . . n, calculate the following: abscissa, BET(i) as the ordinates.
10.4.1 X (i) = relative pressure = P2(i)/Po(i) 10.6 Using a straightedge, draw a line through the linear
10.4.2 Manifold and extra-volume bulb temperatures in region. Deviations from the straight line, if any, should be
kelvins: below the line at low X(i), above the line at high X(i), but not
T 1 ~ i ! 5 T 1 ' ~ i ! 1273.15 (4) apparent within the linear region.
10.7 Determine the slope (S) and intercept (I) of the straight
T 2 ~ i ! 5 T 2 ' ~ i ! 1273.15
line.
T 1x ~ i ! 5 T 1x ' ~ i ! 1273.15 10.7.1 This is preferably done by a least squares calculation,
choosing only those points which fall on the straight line. If a
T 2x ~ i ! 5 T 2x ' ~ i ! 1273.15 point in the linear region is not on the straight line, discard the

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 D3663 − 20
run. It will generally be clear by inspection of the BET plot different materials in seven different laboratories on nine
which points to choose to define the straight line. When the different instruments. Each laboratory performed three repli-
proper choice has been made, deviations of individual points cate analyses on each of the samples over a period of time. All
from the straight line should not exceed about 0.6 % of the samples were degassed at 300 °C under vacuum and evaluated
value of the ordinate. A deviation as large as 1 % is excessive. at nominal P/P0 values of 0.08, 0.11, 0.14, 0.17, and 0.20.
10.8 Calculate Vm, the volume of adsorbate required to Practice E691 was followed for the analysis of the data.
complete one statistical monolayer (cm3 STP/g) Analysis details are in the research report.
V m 5 1/ ~ S1I ! (13) 12.2 Precision—Pairs of tests results obtained by a proce-
10.9 Surface area = 4.353 × Vm. This assumes a value of dure similar to that described in the study are expected to differ
16.2 Å2 (1 Å = 0.1 nm) for the cross-sectional area of a in absolute value by less than 2.772 S, where 2.772 S is the
nitrogen molecule. 95 % probability limit on the difference between two test
NOTE 6—Commercial softwares are available which can perform these results, and S is the appropriate estimate of standard deviation.
calculations and which can assist in determining the appropriate linear
range for the BET plot.
Definitions and usage are given in Terminology E456 and
NOTE 7—A cross-sectional area of 16.2 Å2 for nitrogen is an accepted Practice E177, respectively.
consensus value for standardization and comparison. In actuality, this Test Results 95% Repeatability
value can change from material to material. The assumed cross-sectional 95% Reproducibility
Sample (consensus mean) Interval
Interval m2 (%)
area for the calculations should be reported, especially if it differs from the m2/g m2/g (%)
consensus value. RM8570 10.7 1.1 (10.4) 2.5 (23.0)
RM8571 160 8.9 (5.6) 9.8 (6.1)
11. Report RM8572 289 7.0 (2.4) 11.9 (4.1)

11.1 Report the surface area to three significant figures. 12.3 Bias—This test method is without known bias.
11.2 The report shall include pretreatment, and outgassing
temperatures. 13. Keywords
12. Precision and Bias7 13.1 catalyst; nitrogen adsorption; surface area
12.1 Test Program—An interlaboratory study was con-
ducted in which the surface area was measured on three

7
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D32-1031. Contact ASTM Customer
Service at [email protected].

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