ASTM D3707-89(2005)e1
(Test Method)Standard Test Method for Storage Stability of Water-in-Oil Emulsions by the Oven Test Method
Standard Test Method for Storage Stability of Water-in-Oil Emulsions by the Oven Test Method
SIGNIFICANCE AND USE
This test method indicates the stability of the emulsion during storage and normal usage.
SCOPE
1.1 This test method covers the stability of water-in-oil emulsions when held at a constant elevated temperature.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3707–89(Reapproved 2005)
Standard Test Method for
Storage Stability of Water-in-Oil Emulsions by the Oven Test
Method
This standard is issued under the fixed designation D3707; 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.
´ NOTE—Warning notes were moved into text editorially in May 2005.
1. Scope 5. Apparatus
1.1 This test method covers the stability of water-in-oil 5.1 Convection Oven, meeting the requirements of Specifi-
emulsions when held at a constant elevated temperature. cation E145.
1.2 The values stated in SI units are to be regarded as the 5.2 Graduated Cylinder—A stoppered 100-mL glass cylin-
standard. The values given in parentheses are for information der graduated in 1-mL increments. The stopper should have a
only. vent groove to prevent pressure buildup during the test.
1.3 This standard does not purport to address all of the 5.3 Pipet, 10-mL glass.
safety concerns, if any, associated with its use. It is the 5.4 Microsyringe, 0.05-mLglass with a fixed needle, No. 19
responsibility of the user of this standard to establish appro- gage, point style No. 3.
priate safety and health practices and determine the applica- 5.5 Glass Vials, approximately 30-mL size.
bility of regulatory limitations prior to use.
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 TestMethodforWaterinLiquidPetroleumProducts Vigorous hand shaking or mechanical mixing for 3 to 5 min is
by Karl Fischer Reagent recommended for litre-size containers or less.
E145 Specification for Gravity-Convection and Forced- 6.2 Special difficulties arise in mixing and withdrawing
Ventilation Ovens representative samples from large containers.This is due to the
nature of water-in-oil emulsions which are two-phase systems
3. Summary of Test Method
as distinct from truly homogeneous systems. Vigorous me-
3.1 A 100-mL sample contained in a graduated 100-mL
chanical stirring for an extended period is the best means of
cylinder is placed in a thermostatically controlled oven at 85°C achieving homogeneity. However, for unstable emulsions that
(185°F) for 48 or 96 h. The sample is then examined for the
havebeeninstorageforsometime,thereisnosatisfactoryway
amount of free oil and free water separated. In addition, water to obtain a representative sample.
contents of the sample at specified levels in the upper and
7. Test Method A—48-h Test
lower layers of the sample are also obtained.
7.1 After careful preparation of the sample to obtain homo-
4. Significance and Use
geneity (described in Section 6), transfer 100 mL to a gradu-
4.1 This test method indicates the stability of the emulsion ated 100-mL cylinder. Insert the vented stopper.
during storage and normal usage.
7.2 Placethecylinderinaconvectionovenmaintainedat85
6 1°C (185 6 2°F) for a period of 48 h. Take care to position
the graduated cylinder in the oven generally in the center and
This test method is under the jurisdiction of ASTM Committee D02 on
raise at least 75 mm from the bottom of the oven, to ensure
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.N0 on Hydraulic Fluids. temperature uniformity.
Current edition approved May 1, 2005. Published May 2005. Originally
approved in 1978. Last previous edition approved in 1999 as D3707 – 89 (1999).
DOI: 10.1520/D3707-89R05E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. A “crows-foot” cylinder, British Standard BS 658, may be used.
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D3707–89 (2005)
NOTE 1—Whencarryingoutanumberoftestsatthesametime,arrange TABLE 1 Repeatability and Reproducibility
the cylinders to avoid developing temperature variations in the oven due
Difference in %
to inadequate convection.The number of tests carried out at the same time
Water Content
Free Oil, % Free Water, %
should, for the same reason, also be restricted. Upper Layer Versus
Lower Layer
7.3 Withdraw the cylinder from the oven and allow to stand
Repeatability 1 1 10
Reproducibility 3 1 14
at room temperature, 21 6 3°C (70 6 5°F), for a period of 1
h.
7.4 Observe and record:
7.4.1 The amount of oil separated, percent volume and
10.1.1 Type I—Stable Emulsions (Procedures A and B):
7.4.2 The amount of water separated, percent volume.
7.5 By means of a 10-mL pipet, withdraw aliquots in the
10.1.1.1 The precision of the test method as determined by
following order:
the statistical examination of interlaboratory test results is as
7.5.1 With the pipet tip located exactly at the 80-mL mark,
follows.
slowly withdraw a 10-mL sample and transfer to a small glass
10.1.1.2 Repeatability—The difference between
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