Astm B 328

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This standard test method describes procedures for determining the density, oil content, and interconnected porosity of sintered metal structural parts and oil-impregnated bearings.

This test method covers determination of the density, oil content, and interconnected porosity of sintered bearings and structural parts with or without oil impregnation.

The required apparatus includes an analytical balance, a device for weighing specimens in air and water, a Soxhlet extractor, apparatus for vacuum impregnation of test pieces with oil, beakers, wires, and a thermometer.

Designation: B 328 – 96 (Reapproved 2003)

Standard Test Method for


Density, Oil Content, and Interconnected Porosity of
Sintered Metal Structural Parts and Oil-Impregnated
Bearings1
This standard is issued under the fixed designation B 328; 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 (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope objects, the volume of water displaced by the immersed object


1.1 This test method covers determination of the density, oil is determined by Archimedes principle. For porous P/M parts,
content, and interconnected porosity of sintered bearings and a method is required to seal surface connected pores. If the
structural parts with or without oil impregnation. pores are not sealed or the part is not oil impregnated, the part
1.2 The values stated in SI units are to be regarded as the will absorb some of the water and decrease its buoyancy and
standard. The values in parentheses are for information only. exhibit an erroneously high density.
1.3 This standard does not purport to address all of the 4.2 Density and oil content values are generally contained in
safety concerns, if any, associated with its use. It is the the specifications for oil-impregnated bearings and other self-
responsibility of the user of this standard to establish appro- lubricating P/M parts. Desired lubrication requires sufficient
priate safety and health practices and determine the applica- interconnected porosity and satisfactory oil impregnation of the
bility of regulatory limitations prior to use. porosity.
4.3 For a particular P/M material, the mechanical properties
2. Referenced Documents of P/M structural parts are directly related to their density.
2.1 ASTM Standards: Density values are therefore generally contained in the speci-
B 243 Terminology of Powder Metallurgy2 fications for P/M parts.
D 1217 Test Method for Density and Relative Density
5. Apparatus
(Specific Gravity) of Liquids by Bingham Pycnometer3
D 1298 Test Method for Density, Relative Density (Specific 5.1 Analytical Balance, of sufficient capacity and accurate
Gravity), or API Gravity of Crude Petroleum and Liquid to 0.01 % of the test specimen mass.
Petroleum Products by Hydrometer Method3 5.2 Device for weighing the test piece in air and in liquid
(water); the water is distilled or deionized and preferably
3. Terminology degassed. A wetting agent4 is added to the water, 0.05 to 0.1 %
3.1 Definitions of powder metallurgy (P/M) terms can be by weight, to reduce surface tension effects.
found in Terminology B 243. Additional descriptive informa- 5.3 Soxhlet Extractor, with oil solvent. Extractors may be
tion is available in the Related Material section of Vol 02.05 of purchased from most laboratory supply companies.5
the Annual Book of ASTM Standards. 5.4 Apparatus for vacuum impregnation of the test piece
with oil.
4. Significance and Use 5.5 Beaker and Wires, of various sizes. A wire basket may
4.1 The volume of an arbitrary P/M shape cannot be be used in place of wires (see Figs. 1 and 2).
accurately measured by standard techniques such as by mi- 5.6 Thermometer—Capable of reading temperature in the
crometers or calipers. Since density is mass/volume, a precise range of 10 to 38°C (50 to 100°F) to an accuracy of 0.5°C
method to measure the volume is needed. For nonporous (1°F).

1
This specification is under the jurisdiction of ASTM Committee B09 on Metal
4
Powders and Metal Powder Products and is the direct responsibility of Subcom- Kodak Photo-Flo 200, available from Momentum Graphics, 400 D. Pierce St.,
mittee B09.04 on Bearings. Somerset, NJ 08873, or its equivalent, has been found suitable.
5
Current edition approved April 10, 2003. Published June 2003. Originally Extractors may be purchased from Fisher Scientific, 585 Alpha Drive, Pitts-
approved in 1958. Last previous edition approved in 1996 as B 328 – 96. burgh, PA 15238; Cole-Parmer, 7425 North Oak Ave., Niles, IL 60714; V.W.R., P.O.
2
Annual Book of ASTM Standards, Vol 02.05. Box 15646, Philadelphia, PA 19105-5645; or Thomas Scientific, P.O. Box 99,
3
Annual Book of ASTM Standards, Vol 05.01. Swedesboro, NJ 08085-6099.

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

1
B 328 – 96 (2003)
not more than 7 kPa (2 in. mercury) pressure for 30 min. Then
permit the pressure to increase to atmospheric pressure and the
specimen to remain immersed in oil 20 to 65 cSt (100 to 300
SSU) 38°C (100°F) at room temperature and pressure for 10
min.
7.3.2 Immerse the specimen in oil, viscosity of 20 to 65 cSt
(100 to 300 SSU) at 38°C (100°F), hold at a temperature of
82°C 6 5°C (180°F 6 10°F) for at least 4 h, and then cool to
room temperature by immersion in oil at room temperature.
7.4 To weigh the specimen in water, select a fine wire for
a. Twisted wire arrangement b. Basket support arrangement supporting the specimen. Suspend the wire from the beam
FIG. 1 Methods for Holding Test Specimen When Weighing in hook, while the specimen is immersed in a beaker of distilled
Water water. Support the beaker of water over the pan of the balance,
using a suitable bridge. The container of water may also be
5.7 Lubricant, of 20 to 65 cSt (100 to 300 SSU) at 38°C supported below the balance for weighing specimens if the
(100°F). balance has a lower beam hook for this purpose. See Fig. 2b.
Use a wetting agent (in the amount of 0.05 to 0.1 % by weight)
6. Test Specimen to reduce the effects of surface tension. The recommended
diameter of wire (copper or stainless steel) to be used for
6.1 The specimen mass shall be a minimum of 1.0 g.
various weight range is as follows:
Several specimens may be used to reach the minimum mass.
less than 50 g − 0.12 mm (0.005 in.)
7. Procedure 50 to less than 200 g − 0.25 mm (0.010 in.)
200 to less than 600 g − 0.40 mm (0.015 in.)
7.1 Using an analytical balance, obtain the mass of the as
600 g and greater − 0.50 mm (0.020 in.)
received oil-containing specimen (Mass J), the oil-free speci-
In place of attaching the specimen on a wire, the use of a
men (Mass A), and the fully impregnated specimen (Mass B).
wire basket suspended in water may be used as an alternate
These, and all subsequent weighing, should be to 0.01 % of the
method (see Fig. 1b).
mass of the part, for example:
7.5 Twist the wire around the specimen and suspend it from
Specimen Mass, g Balance Sensitivity, g
the beam hook so that the specimen is completely immersed in
less than 10 0.0001 the water. The water should cover the specimen by at least 6
10 to less than 100 0.001 mm (0.25 in.) and the wire twist should be completely
100 to less than 1000 0.01
1000 to less than 10 000 0.1 submerged. Immersion should be to the same point each time.
Take care to ensure that no air bubbles adhere to the specimen
7.2 To determine Mass A, remove any oil from the samples or to the wire. If a wire basket is used as an alternate method,
by extracting it in a Soxhlet apparatus of suitable size using completely immerse the wire basket in the water.
toluol or petroleum ether as a solvent. After extracting for
7.6 Weigh the specimen and wire in water. This is Mass C.
approximately 1 h, remove the residual solvent by heating
If a wire basket is used as an alternate method, weigh the
samples 1 h at 120°C (250°F) and weigh upon cooling.
specimen and wire basket in water.
Continue alternate extractions and drying until the dry mass in
7.7 Remove the specimen and reweigh the wire in water
air is constant to 0.05 % of the mass of the part.
immersed to the same point as before. This is Mass E. Some
7.2.1 For large parts or for a faster method, but not as
balances are capable of being tared automatically, which
accurate and with no concern for subsequent metallurgical
eliminates the need for reweighing the wire for correction. The
properties, the oil can be removed by heating the specimen in
mass of the oil impregnated specimen in water with the mass
a protective atmosphere in the temperature range of 430 to
of wire tared is Mass F. Excess oil should be removed from the
650°C (800 to 1200°F). This method may be used if agreed
surface of the specimen before weighing. Care should be taken
upon by both parties. The selection of a proper burnout
not to remove oil from the porosity of the part. Water density,
temperature may be critical in the case of sintered 90/10 Cu/Sn
Dw, is found in Table 1. Measure the temperature of the water
materials, depending upon the sintering temperature and time
to the nearest 1°C.
used by the fabricator. The normal sintering temperature range
for bronze is 815 to 870°C (1500 to 1600°F), depending on the 7.7.1 If a wire basket is used as the alternate method, follow
desired shrinkage, strength, and porosity relationships. This the same procedure but substitute the basket for the wire.
method is also applicable to sintered aluminum materials if the 7.8 For oil content and interconnected porosity, determine
temperature does not exceed 540°C (1000°F). the density of the impregnant, which is (Do). Oil content is
7.3 For the purpose of determining the mass of oil- defined as the percent oil content by volume in the part as
impregnated specimens in air (Mass B) or in water (Mass C), received. The interconnected porosity is the percent oil content
either of the following two methods may be used to impregnate by volume in the part as it is impregnated under specific
the test specimen. The vacuum method is preferred. laboratory conditions.
7.3.1 At room temperature, using a suitable evacuating NOTE 1—Typical density of petroleum-type lubricants is 0.880 g/cm3
method, reduce the pressure over the immersed specimen to and for synthetic lubricants it ranges from 0.910 to 1.000 g/cm3 . Refer to

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B 328 – 96 (2003)

a. Weighing a small specimen within the balance b. Weighing a large specimen below the balance
FIG. 2 Methods for Weighing in Water

TABLE 1 Effect of Water Temperature on Water DensityAB


Temperature Density
S A
D 5 B 2 C 1 E Dw 5 D SA
B 2 ~C 2 E!
Dw D (1)

°C
15
(°F)
(59.0)
g/cm3
0.9991
A
S D
D 5 B 2 F Dw (2)
16 (60.8) 0.9989
17 (62.6) 0.9988
18 (64.4) 0.9986 where:
19 (66.2) 0.9984 D = density, g/cm3,
20 (68.0) 0.9982
21 (69.8) 0.9980
A = mass in air of oil-free specimen, g,
22 (71.6) 0.9978 B = mass of oil-impregnated specimen, g,
23 (73.4) 0.9975 C = mass of oil-impregnated specimen and wire in water,
24 (75.2) 0.9973
g,
25 (77.0) 0.9970
26 (78.8) 0.9968 E = mass of wire in water, g,
27 (80.6) 0.9965 Dw = density of water at the immersion temp, g/cm3, and
28 (82.4) 0.9962 F = mass of oil-impregnated specimen in water, with
29 (84.2) 0.9959
30 (86.0) 0.9956
mass of wire tared.
A
Handbook of Chemistry and Physics,“ Absolute Density of Water Table,” 65th
8.2 Calculate the wet density of bearings supplied fully
Edition, p F-4. impregnated with lubricant using Eq 3 or Eq 4 (alternative):

S D
B
Metrological Handbook 145, “Quality Assurance for Measurements,” National
Institute of Standards and Technology, 1990, pp. 9, 10.
B
D 5 B 2 C 1 E Dw (3)

Test Method D 1217 or Practice D 1298 for determining the density of the
lubricants.
B
S
D 5 B 2 F Dw D (4)

8. Calculation where:
8.1 Calculate the density of structural parts using Eq 1 or Eq D = density, g/cm3,
B = mass of oil-impregnated specimen, g,
2 (alternative):

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B 328 – 96 (2003)

C = mass of oil-impregnated specimen and wire in water, where:


g, P1 = oil content by volume, as received, %,
E = mass of wire in water, g, J = mass of oil-impregnated specimen as received, g,
Dw = density of water at the immersion temp, g/cm3, and Do = density of oil, g/cm3,
F = mass of oil-impregnated specimen in water, with Dw = density of water at the immersion temperature,
mass of wire tared, g. g/cm3,
8.3 Calculate the interconnected porosity and the oil content A = mass in air of oil-free specimen, g,
by volume using Eq 5, Eq 6, or Eq 7 (alternative). B = mass of oil impregnated specimen, g,
8.3.1 Interconnected Porosity: C = mass of oil impregnated sample immersed in water,

F G
g,
B2A
P5 3 100 Dw (5) E = mass of wire in water, g, and
~ B 2 C 1 E ! 3 Do F = mass of oil impregnated specimen in water with mass
of wire tared, g.
P5 F B2A
~ B 2 ~ C 2 E ! 3 Do
3 100 Dw G (6)
9. Precision and Bias
P5 F
B2A
~ B 2 F ! 3 Do
3 100 Dw G (7) 9.1 For ferrous and copper base sintered parts, the repeat-
ability interval, (r), is 0.05 g/cm3 for dry or wet density. It is 2.0
where: percentage points for porosity. Duplicate results from the same
P = interconnecting porosity by volume, %, laboratory should not be considered suspect at the 95 %
A = mass in air of oil-free specimen, g, confidence level unless they differ by more than (r).
B = mass of oil-impregnated specimen, g,
C = mass of oil-impregnated sample immersed in water, 9.2 For ferrous and copper base sintered parts, the repro-
g, ducibility interval (R) is 0.06 g/cm3 for dry or wet density, and
E = mass of wire in water, g, 4.0 percentage points for porosity. These results from two
Do = density of the oil, g/cm3, different laboratories should not be considered suspect at the
F = mass of oil impregnated specimen in water with mass 95 % confidence level unless they differ by more than (R).
of wire tared, g, and 9.3 There is no estimate of bias because there is no accepted
Dw = density of water at the immersion temperature, porous reference material. A test program using fully dense
g/cm3. silicon as a reference is being undertaken.
8.3.2 Oil Content by Volume as Received—Use Eq 8 and 9,
or Eq 10 (alternative): 9.4 These data are based upon the identical sample checked
at six different laboratories.
P1 5 F J2A
~ B 2 C 1 E ! 3 Do
3 100 Dw G (8)
10. Keywords
P1 5 F J2A
@B 2 ~C 2 E!# Do
3 100 Dw G (9) 10.1 density; interconnected porosity; oil content; oil-

F G
J2A impregnated bearings; P/M; powder metallurgy; sintered
P1 5 3 100 Dw (10) metal; structural parts
~ B 2 F ! 3 Do

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