ASTM D3709-89(1999)
(Test Method)Standard Test Method for Stability of Water-in-Oil Emulsions Under Low to Ambient Temperature Cycling Conditions
Standard Test Method for Stability of Water-in-Oil Emulsions Under Low to Ambient Temperature Cycling Conditions
SCOPE
1.1 This test method is intended to indicate the stability of water-in-oil emulsions when subjected to temperature cycling changes between ambient temperature and-18°C (0°F).
1.2 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems 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.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D3709–89(Reapproved 1999)
Standard Test Method for
Stability of Water-in-Oil Emulsions Under Low to
Ambient Temperature Cycling Conditions
This standard is issued under the fixed designation D3709; 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 5. Apparatus
1.1 This test method is intended to indicate the stability of 5.1 Cold Box—Athermostaticallycontrolledfreezerorcold
water-in-oil emulsions when subjected to temperature cycling box capable of being maintained at−18 6 1.5°C (0 6 3°F).
changes between ambient temperature and –18°C (0°F). 5.2 Graduated Cylinder—A stoppered 100-mL glass cylin-
1.2 This standard does not purport to address all of the der graduated in 1.0-mL increments. The stopper should have
safety concerns, if any, associated with its use. It is the a vent groove to prevent vacuum or pressure build-up during
responsibility of the user of this standard to establish appro- the test.
priate safety and health practices and determine the applica- 5.3 Pipet, 10-mL glass.
bility of regulatory limitations prior to use. 5.4 Microsyringe,0.05-mLglasswithafixedneedle,No.19
1.3 The values stated in SI units are to be regarded as the gage, point style No. 3.
standard. The values given in parentheses are for information 5.5 Glass Vials, approximately 30-mL size.
only.
6. Preparation of Sample
2. Referenced Documents
6.1 To ensure uniformity of the sample, it should be mixed
2.1 ASTM Standards: thoroughly before removing the quantity required for the test.
D1744 Test Method for Water in Liquid Petroleum Prod- Vigorous hand shaking or mechanical mixing for 3 to 5 min is
ucts by Karl Fischer Reagent recommended for litre-size containers or less.
6.2 Special difficulties arise in mixing and withdrawing
3. Summary of Test Method
representativesamplesfromlargecontainers.Thisisduetothe
3.1 A 100-mL sample contained in a graduated 100-mL nature of water-in-oil emulsions that are two-phase systems as
cylinderisplacedinacoolingboxat−18°C(0°F)for16hand
distinct from truly homogeneous systems. Vigorous mechani-
thenallowedtostandatroomtemperaturefor8h.Thiscycling cal stirring for an extended period is the best means of
procedure is repeated to give a total of nine cycles, except that
achieving homogeneity. However, for unstable emulsions that
the fifth cycle is one of 64 h at−18°C (0°F), 8 h at room havebeeninstorageforsometimethereisnosatisfactoryway
temperature. At the completion of the cycling procedure the
to obtain a representative sample.
sample is examined for the amount of free oil and free water
7. Procedure
separated.Inaddition,watercontentsofthesampleatspecified
levels in the upper and lower layers of the sample are also 7.1 After careful preparation of the sample to ensure homo-
obtained. geneity (described in Section 6), transfer 100 mL to a gradu-
ated 100-mL cylinder. Insert the vented stopper.
4. Significance and Use
7.2 Place the cylinder in the cold box at−18 6 1.5°C (0 6
4.1 This test method indicates the ability of the emulsion to
3°F) for a period of 16 h.Withdraw the cylinder from the cold
withstand mild to moderately severe winter conditions of use box and allow to stand at room temperature, 21 6 3°C (70 6
and storage. Generally this significance would be limited to
5°F), for a period of 8 h.
conditionswheretheemulsionreachesaminimumtemperature 7.3 Repeat the cycling procedure as in 7.2 for three more
of−18°C (0°F).
cycles.
7.4 Replace the cylinder in the cold box for a period of 64
h. Withdraw and allow to stand at room temperature for 8 h.
This test method is under the jurisdiction of ASTM Committee D-2 on
7.5 Repeat the cycling procedure as in 7.2 for four more
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.N0.02on Industrial Applications. cycles, except that during the final cycle, the period at room
Current edition approved Oct. 27, 1989. Published December 1989. Originally
temperature is limited to 3 h instead of 8 h before making
published as D3709–78. Last previous edition D3709–83.
observations.
Annual Book of ASTM Standards, Vol 05.01.
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D3709
7.6 Observe and record the following: 9.1.1.2 Repeatability—The difference between successive
7.6.1 The amount of oil separated, percent volume and results obtained by the same operator with the same apparatus
7.6.2 The amount of w
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