Astm D892 - 10
Astm D892 - 10
Astm D892 - 10
Designation: D892 – 10
Designation: 146/2000
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D892 – 10
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D892 – 10
cylinders with pouring spouts by cutting them off below the spouts. The copper tubing placed around the inside circumference of the
cut surface is to be smoothed before use by fire polishing or grinding. cold bath so that the volume measurement is made at approxi-
NOTE 3—Gas diffusers may be attached to air-inlet tubes by any mately 24°C (75°F). Precautions are to be taken to avoid leaks
suitable means. A convenient arrangement is shown in Fig. 2.
NOTE 4—It may be necessary to confirm the volume of the cylinder.
at any point in the system.
6.2 Test Baths, large enough to permit the immersion of the NOTE 8—Alternatively, a 1 L cylinder (with 10 mL graduation marks)
full of water is inverted in a tall, large beaker also filled with water. There
cylinder at least to the 900-mL mark and capable of being
should be no air bubbles inside. Air leaving the copper loop in the bath is
maintained at temperatures constant to 0.5°C (1°F) at 24°C connected below the cylinder. When the test is started, air will flow into
(75°F) and 93.5°C (200°F), respectively. Both bath (Note 6) the cylinder, displacing the water. At the end of the test, the volume of air
and bath liquid shall be clear enough to permit observation of in the cylinder is measured by equalizing the water levels inside and
the graduations on the cylinder. outside the cylinder. Alternatively, the total volume of air passed would be
the difference between the final and the initial volumes of water in the
NOTE 5—Air baths may also be utilized for heating purposes. Limited cylinder.
data has shown that both liquid and air baths give equivalent results. NOTE 9—A wet test meter calibrated in hundredths of a litre is suitable.
However, the precision estimates given in Section 13 are based on using
only liquid baths.3 6.4 Timer, graduated and accurate to 1 s or better.
NOTE 6—Heat-resistant cylindrical glass jars approximately 300 mm 6.5 Temperature Sensing Device, capable of covering the
(12 in.) in diameter and 450 mm (18 in.) in height make satisfactory baths. temperature range from at least 20 to 100°C, with an accuracy
6.3 Air Supply, from a source capable of maintaining an air of 60.5°C. A thermometer having a range as shown below and
flow rate of 94 6 5 mL/min through the gas diffuser. The air conforming to the requirements as prescribed in Specification
shall be passed through a drying tower 300 mm in height E1 or specifications for IP thermometers has been found
packed as follows: just above the constriction place a 20-mm suitable to use:
layer of cotton, then a 180-mm layer of indicating desiccant, Temperature Thermometer
Range ASTM No. IP
and a 20-mm layer of cotton. The cotton serves to hold the 20 to 102°C 12C 64C
desiccant in place. Refill the tower when the indicating
desiccant begins to show presence of moisture. A flowmeter 7. Reagents and Materials
sensitive to the required tolerances can be used to measure the 7.1 Purity of Reagents—Reagent grade chemicals shall be
air flow (Note 7). used in all cases. Unless indicated otherwise, it is intended that
all reagents conform to the specifications of the committee on
NOTE 7—A manometer type flowmeter, in which the capillary between
the two arms of the U-tube is approximately 0.4 mm in diameter and 16 Analytical Reagents of the American Chemical Society where
mm in length, and in which n-butylphthalate is the manometric liquid, is such specifications are available.4 Other grades may be used,
suitable. provided it is first ascertained that the reagent is of sufficiently
6.3.1 The total volume of air leaving the foaming test high purity to permit its use without lessening the accuracy of
apparatus shall be measured by a volume measuring device the determination.
(Note 9) capable of accurately measuring gas volumes of about
4
470 mL. The air shall be passed through at least one loop of 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 Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
3
Supporting data have been filed at ASTM International Headquarters and may and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
be obtained by requesting Research Report RR:D02-1516. MD.
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D892 – 10
7.2 Acetone—(Warning—Extremely flammable, vapors NOTE 12—Certain samples may contain ingredients which may not be
can cause a flash fire). adequately removed by this process and, because these can affect the next
7.3 Compressed Air, hydrocarbon free and dry to a dew test, more rigorous cleaning may be required; this is recommended. When
alternate diffuser cleaning methods are used certain cautions should be
point of −60°C or lower. observed: (1) Non-metallic diffusers may have absorbed as well as
NOTE 10—If the source of compressed air is ensured to the stated adsorbed these interfering ingredients or the cleaners, or both, and this
specifications, the drying tower in 6.3 may not be necessary. shall be considered before proceeding to the next test. (2) So that all tests
performed start off under the same circumstances, when alternate diffuser
7.4 Heptane—(Warning—Flammable, vapor harmful). cleaning methods are used, the final rinsing process shall be as detailed in
7.5 Propan-2-ol—(Solvents with equivalent cleaning and 9.1.2. (3) See also Note 1.
solvency characteristics may be substituted for propan-2-ol.)
7.6 Toluene (Methylbenzene)—(Solvents with equivalent 10. Procedure
cleaning and solvency characteristics may be substituted for
10.1 Sequence I—Without mechanical shaking or stirring,
toluene.)
decant approximately 200 mL of sample into a beaker (see
10.1.1). Heat to 49 6 3°C and allow to cool to 24 6 3°C. See
8. Hazards
Option A for stored sample (see 10.5). Each step of the
8.1 (Warning—Users of this test method shall be trained procedure described in 10.3 and 10.4, respectively, shall be
and familiar with all normal laboratory practices, or under the carried out within 3 h after completion of the previous step. In
immediate supervision of such a person. It is the responsibility 10.5.1, the test shall be carried out as soon as compatible with
of the operator to ensure that all local legislative and statutory the temperature specification and not more than 3 h after
requirements are met.) immersion of the cylinder in the 93.5°C (200°F) bath.
8.2 (Warning—Cleaning solvents have flash points lower 10.1.1 If a sample arrives in the lab and it has been
than ambient temperatures. Avoid the possibility of fire or determined that it is at or above 49 6 3°C, the heating step in
explosion.) 10.1 may be eliminated. Heating the sample to 49 6 3°C in
8.3 (Warning—The fumes from the test oil and the bath 10.1 is intended to remove any thermal history before proceed-
shall be vented in a manner compatible with local government ing, which is not an issue for samples arriving in the lab
regulations.) already at or above 49 6 3°C.
8.4 (Warning—Some apparatus assemblies can have as
much as 20 L of heat transfer oil at 93.5°C. Therefore, in the 10.2 Pour the sample into the 1000-mL cylinder until the
event of breakage of the containing vessel, provisions for liquid level is at the 190-mL mark. Visually estimate the level
suitable containment of the spill is advisable.) to be within 5 mL. Immerse the cylinder at least to the 900-mL
mark in the bath maintained at 24 6 0.5°C (75 6 1°F). When
the oil has reached the bath temperature, insert the gas diffuser
9. Preparation of Apparatus
and the air-inlet tube with the air source disconnected, and
9.1 Thorough cleansing of the test cylinder and air-inlet permit the gas diffuser to soak for about 5 min. Connect the
tube is essential after each use to remove any additive air-outlet tube to the air volume measuring device. At the end
remaining from previous tests which can seriously interfere of 5 min, connect to the air source, adjust the air flow rate to
with results of subsequent tests. 94 6 5 mL/min, and force clean dry air through the gas diffuser
9.1.1 Cylinder—Rinse the cylinder with heptane. for 5 min 6 3 s, timed from the first appearance of air bubbles
(Warning—Flammable, vapor harmful.) Wash the cylinder rising from the gas diffuser. At the end of this period, shut off
with a suitable detergent. Rinse the cylinder, in turn, with the air flow by disconnecting the hose from the flow meter and
distilled water, then acetone (Warning—Extremely flam- immediately record the volume of foam; that is, the volume
mable, vapors can cause a flash fire) and dry in a current of the between the oil level and the top of the foam. The total air
compressed air or in a drying oven. Interior walls that drain the volume which has passed through the system shall be 470 6 25
water cleanly, that is without drops forming, are adequately mL. Allow the cylinder to stand for 10 min 6 10 s and again
cleaned. record the volume of foam (see 10.2.1).
NOTE 11—Certain detergents are notorious for adhering to glass; 10.2.1 In cases after the air supply has been disconnected,
therefore, it is important to realize that such a circumstance can affect the where the foam collapses to 0 mL before the 10 min settling
test result. Several rinsings with water and acetone may be required. time has elapsed, the test may be terminated and the foam
9.1.2 Gas Diffuser and Air Tube—Clean the gas diffuser stability result recorded as 0 mL.
with toluene (solvents with equivalent cleaning and solvency 10.3 Sequence II—Pour a second portion of sample into a
characteristics may be substituted for toluene.) and heptane. cleaned 1000-mL cylinder until the liquid level is at the
Immerse the gas diffuser in about 300 mL of toluene. Flush a 180-mL mark. Visually estimate the level to be within 5 mL.
portion of the toluene back and forth through the gas diffuser Immerse the cylinder at least to the 900-mL mark in the bath
at least five times with vacuum and air pressure. Repeat the maintained at 93.5 6 0.5°C (200 6 1°F). When the oil has
process with heptane. After the final washing, dry both the tube reached a temperature of 93 6 1°C, insert a clean gas diffuser
and the gas diffuser thoroughly by forcing clean air through and air-inlet tube and proceed as described in 10.2, recording
them. Wipe the outside of the air inlet tube, first with a cloth the volume of foam at the end of the blowing and settling
moistened with heptane, then a dry cloth. Do not wipe the gas periods. In cases where 10.2.1 applies, the test procedure may
diffuser. continue to Sequence III.
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D892 – 10
10.4 Sequence III—Collapse any foam remaining after the
test at 93.5°C (200°F) (10.3), by stirring. Cool the sample to a
temperature below 43.5°C (110°F) by allowing the test cylin-
der to stand in air at room temperature, then place the cylinder
in the bath maintained at 24 6 0.5°C (75 6 1°F). After the oil
has reached bath temperature, insert a cleaned air-inlet tube and
gas diffuser and proceed as described in 10.2, recording the
foam value at the end of the blowing and settling periods. (See
10.2.1.)
10.5 Some lubricants with modern additives can pass their
foam requirements when blended (with the antifoam properly
dispersed in small particle sizes) but fail to meet the same
requirements after two or more weeks’ storage. (It appears that
the polar dispersant additives have the potency to attract and
hold antifoam particles, such that the apparent increased
antifoam size results in decreased effectiveness to control foam
in Test Method D892.) However, if the same stored oil is
merely decanted and poured into engines, transmissions, or FIG. 3 Precision Chart—Repeatability
gear boxes and those units operated for a few minutes, the oil
again meets its foam targets. Similarly, decanting the stored oil 12. Report
into a blender, followed by agitation as described for Option A 12.1 Report the data in the following manner:
(see 10.5.1), redisperses the antifoam held in suspension and Foaming Tendency ASTM Foam Stability ASTM D892
the oil again will give good foam control in Test Method D892. D892 IP 146 IP 146
For such oils, Option A can be used. On the other hand, if the Foam Volume, mL, at end of Foam Volume, mL, at end of
Test 5-min blowing period 10-min settling period
antifoam is not dispersed into sufficiently small particles when As received:
the oil is blended, the oil cannot meet its foam requirements. If Sequence I ... ...
Sequence II ... ...
this freshly blended oil were vigorously stirred according to Sequence III ... ...
Option A, it is very possible that the oil would then meet its After agitation:
foam targets whereas the plant blend would never do so. (Option A, 9.5.1)
Sequence I ... ...
Therefore, it is inappropriate and misleading to apply Option A Sequence II ... ...
for quality control of freshly made blends. Sequence III ... ...
10.5.1 Option A—Clean the container of a 1-L (1-qt), 12.2 For the purpose of reporting results, when the bubble
high-speed blender using the procedure given in 9.1.1. Place layer fails to completely cover the oil surface and a patch or
500 mL of sample measured from 18 to 32°C (65 to 90°F) into eye of clear fluid is visible, the value shall be reported as nil
the container, cover, and stir at maximum speed for 1 min. foam.
Because it is normal for considerable air to be entrained during
this agitation, allow to stand until entrained bubbles have 13. Precision and Bias 5
dispersed and the temperature of the oil has reached 24 6 3°C 13.1 Precision—The precision values in this statement were
(75 6 5°F). Within 3 h following the agitation (solvents with determined in a cooperative laboratory program.6
equivalent cleaning and solvency characteristics may be sub- 13.1.1 Repeatability—The difference between successive
stituted for toluene), start with testing as specified in 10.2. results obtained by the same operator with the same apparatus
under constant operating conditions on identical test material
NOTE 13—In case of viscous oils, 3 h can be insufficient time to would, in the long run, in the normal and correct operation of
disperse the entrained air. If a longer time is required, record the time as the test method exceed the following values in only one case in
a note on the results.
twenty (see Fig. 3).
13.1.2 Reproducibility—The difference between two single
11. Alternative Procedure
and independent results obtained by different operators work-
11.1 For routine testing a simplified testing procedure can ing in different laboratories on identical test material would, in
be used. This procedure differs from the standard method in the long run, exceed the following values in only one case in
only one respect. The total air volume used during the 5-min twenty (see Fig. 4).
blowing period is not measured after the air has passed through NOTE 14—The dashed lines in Fig. 3 and Fig. 4 are for foam stability
the gas diffuser. This eliminates the volume measuring equip- of Sequence III and the solid lines are for foam height for Sequences I, II,
ment and the airtight connections necessary to carry the exit air
from the graduated cylinder to the volume measuring device,
5
but requires that the flowmeter be correctly calibrated and that Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1244.
the flow rate be carefully controlled. Results obtained by this 6
Filed at ASTM International Headquarters and may be obtained by requesting
procedure shall be reported as D892 – IP 146 (Alternative). Research Report RR:D02-1007.
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D892 – 10
and III and foam stability for Sequences I and II.
14. Keywords
14.1 foam (foaming)
ANNEX
(Mandatory Information)
A1. TEST FOR MAXIMUM PORE DIAMETER AND PERMEABILITY OF GAS DIFFUSERS
(BASED ON TEST METHOD E128)
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D892 – 10
bubble is recognized by being followed by a succession of where:
additional bubbles. Read the water level in both legs of the p = water in the manometer, mm.
manometer and record the difference p. The uniformity of A1.2.1.2 Calibration of diffusers have been found to be a
distribution of pores approaching maximum pore size may be critical factor in this test.7
observed by gradually increasing the air pressure and noting A1.2.2 Permeability—Connect the clean, dry diffuser with a
the uniformity with which streams of bubbles are distributed controllable source of clean, dry, compressed air, again using a
over the surface. 1-m length of 8-mm-bore tubing, and place it in a filtering flask
A1.2.1.1 Calculate the maximum pore diameter, D, in connected to a suitable flowmeter using a further 0.5-m length
micrometres, as follows: of tubing as shown in Fig. A1.2. Adjust the pressure differential
(1) For non-metallic diffusers and water as the diffuser to 2.45 kPa (250 mm of water) and measure the rate of flow of
medium: air through the gas diffuser in millilitres per minute. Depending
D 5 29 225/~p 2 100! (A1.1) on the sensitivity of the flowmeter used, this observation may
be made for a suitably longer period and the average flow rate
where: per minute recorded.
p = mm of water.
(2) For metallic diffusers and propan-2-ol as the diffuser
medium: 7
Supporting data have been filed at ASTM International Headquarters and may
D 5 8930/~p 2 80! (A1.2) be obtained by requesting Research Report RR:D02-1369.
APPENDIXES
(Nonmandatory Information)
X1.1 Helpful Hints X1.1.9 The total volume of the air passing through the
X1.1.1 The test should be performed exactly as described to system should be measured to 470 6 25 mL. Without this step,
obtain good results. there is no way of ascertaining that the system is airtight.
X1.1.2 Norton stone diffusers are known to be unreliable X1.1.10 It is recommended that the stopwatches be cali-
regarding their porosity and permeability; hence, new stones brated against a national standard at least once a year. Annex
(as well as the metal diffusers) need to be checked in A3 (Timer Accuracy) of Test Method D445 is a good source for
accordance with Annex A1. guidance on how to check the timers for accuracy.
X1.1.3 The diffusers should be checked periodically for X1.1.11 If using Option A, all entrained air bubbles after
porosity and permeability, depending upon the usage; checking stirring should be dispersed before testing.
is recommended at least once a week. Out of specification X1.1.12 It is misleading and inappropriate to apply Option
diffusers are a major cause of inaccuracy in this test method. A for quality control of freshly made blends, or comparing/
X1.1.4 The connection between the gas diffusers and the air reporting Option A and regular foam test results.
inlet tubes should be airtight. X1.1.13 If the alternative procedure is used for measure-
X1.1.5 The inlet air should be dried by passing through a ments, the data should not be reported as that obtained by Test
desiccant drying tower. The indicator desiccant needs to be Method D892.
changed when it shows the presence of moisture by changing
X1.1.14 In 6.1, verify the distance between inside bottom of
its color from blue to pink.
the cylinder and the 1000 mL graduation mark.
X1.1.6 If a thermometer is used as the temperature sensing
device (see 6.5), thermometer calibration should be checked at X1.1.15 In 6.1, a diffuser centering washer is used to ensure
least annually against a master thermometer. For other tem- the diffuser head is centered within the cylinder to eliminate
perature sensing devices, checking the calibration at least wall interference with foam generation and expansion during
annually against a traceable source is also recommended. and after the blowing period. This is particularly helpful when
X1.1.7 Thorough cleaning of the test cylinder and the air dark fluids are tested or lighting conditions or darkened bath
inlet tube is essential after each use to remove any residual liquids make centering difficult.
additive from the previous analysis. X1.1.16 In 6.1, hold the cylinders in an upright position by
X1.1.7.1 The cylinders are cleaned with heptane, a suitable use of a suitable device. If the cylinders are not vertical or
detergent, distilled water, acetone, and dried with air or in an move during the test, or both, foam level errors can be
oven, in sequence. increased.
X1.1.7.2 The gas diffusers are cleaned at least five times X1.1.17 In 9.1.2, avoid touching the diffusers with one’s
with toluene, heptane, and clean dry air in sequence. hands.
X1.1.8 Oil or water baths must be used to control testing X1.1.18 In 10.2-10.4, verify that the sample has reached the
temperatures within 0.5°C (1°F). bath temperature before starting the measurements.
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D892 – 10
X2.1 An Interlaboratory Study (ILS) was organized to moving oil residue and varnish from glassware.
improve precision of Test Method D892. Twelve laboratories X2.4.1 After cleaning the cylinder according to 9.1.1, wash
participated in the ILS. the cylinder interior with commercial cleaning agent. Rinse
X2.1.1 Participating laboratories included ten user labora- with warm water and allow to thoroughly dry.
tories, one commercial test laboratory, and one foam test NOTE X2.4—For more effective cleaning, periodically fill the cylinder
instrument manufacturer’s laboratory. Eight of the laboratories with commercial cleaning agent and allow to soak for 30 m. Rinse with
used liquid baths and four used air baths. All laboratories used warm water and allow to dry.
only new and calibrated metal diffusers, and all laboratories
were equipped with the same type of device for measuring the X2.5 Sequence I (see 10.1)—Slowly invert the container of
air actually passing through the diffuser and fluid as schemati- test fluid 180° and return to upright 20 times (2 s minimum for
cally shown in Fig. X2.1. each inversion cycle) by hand (or rotate by machine). Do not
shake container. Follow the remainder of 10.1-10.4. However,
NOTE X2.1—Any device for precisely measuring the actual volume
Option A (10.5) shall not be used.
required for the test can be used.
X2.1.2 Five samples consisting of three engine oil types, a X2.6 Do not use the alternative procedure shown in 11.1.
base oil, and a commercially available reference oil were NOTE X2.5—Alternative procedures, which depend on measuring rate
analyzed in duplicate. of incoming air (gas) flow rather than the total volume of air (gas) flow
that has passed through the diffuser, have been found questionable as a
X2.2 Some deviations from Test Method D892 were result of undetected leakage of the tubing connecting the air (gas) to the
specified. The main deviations included: diffuser or undetected changes in the porosity of the diffusers.
X2.2.1 Samples were upended 20 times before being put
X2.7 The following precision and bias statements were
into the test cylinder.
obtained from this ILS:8
NOTE X2.2—This differs from 10.1 of the test method in specifying X2.7.1 Repeatability—The difference between successive
effective and precisely repeatable mixing of the sample rather than the
highly variable and vigorous mixing specified in Option A.
results obtained by the same operator with the same apparatus
under constant operating conditions on identical test material
X2.2.2 A diffuser centering washer was used to ensure the would, in the long run, in the normal and correct operation of
diffuser head was accurately centered within the glass cylinder the test method, exceed the values shown below and in Fig.
during the 5-min blowing period. This is shown in Fig. X2.2. X2.3 in only 1 case in 20.
X2.2.3 There was no more than a 1-h delay after heating. Sequence Repeatability
10.1 allows up to a 3-h delay. I 0.10 (x + 55)
X2.2.4 An effective commercial glass cleaning agent was II 0.10 (x + 44)
III 0.15x
specified in addition to the cylinder cleaning steps in 9.1.1 of
the test method to ensure cylinders were thoroughly cleaned of where x = the determined value.
oil residue prior to each test run. X2.7.2 Reproducibility—The difference between successive
X2.2.5 The procedure for Option A for blending was not results obtained by different operators with different appara-
used. tuses in different laboratories on identical test material would,
X2.2.6 The alternative procedure (11.1 of the test method) in the long run, in the normal and correct operation of the test
was not used. Instead, it is required to measure the air passing method, exceed the values shown in below and in Fig. X2.4 in
through the diffuser and test fluid with an exit air volume only 1 case in 20.
measuring device. Sequence Reproducibility
I 0.29 (x + 55)
NOTE X2.3—For operators looking to improve consistency and test II 0.26 (x + 44)
precision, the remaining sections of Appendix X2 offer further clarifica- III 0.44x
tion of techniques from the ILS not presently in Test Method D892.
Complete details of the ILS are described in an ASTM Research Report where x = the determined value.
being prepared to be submitted to ASTM International Headquarters. X2.7.3 Bias—Since there is no accepted reference material
suitable for determining the bias for the procedure for measur-
X2.3 Diffuser Centering Washer—Thin washer (1 mm ing foaming characteristics in Appendix X2 of Test Method
thick) whose overall diameter is slightly smaller than the D892, bias cannot be determined.
cylinder diameter and whose center diameter is 4 mm larger
than the diameter of the diffuser.
8
Supporting data have been filed at ASTM International Headquarters and may
X2.4 Commercial Glass Cleaning Agent—capable of re- be obtained by requesting Research Report RR:D02-1618.
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D892 – 10
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D892 – 10
SUMMARY OF CHANGES
Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D892–06´1) that may impact the use of this standard.
(1) Updated 3.2.2.1, 4.1, 6.5, 10.1-10.4, and X1.1.6. (4) Deleted footnotes that identified the sole source of equip-
(2) Added 4.2, 4.3, 10.1.1, and 10.2.1. ment vendor.
(3) Harmonized definitions to match other D02.06 standards.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
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of infringement of such rights, are entirely their own responsibility.
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