ASTM D3709-89(2005)e1

Standard Test Method for Stability of Water-in-Oil Emulsions Under Low to Ambient Temperature Cycling Conditions

SIGNIFICANCE AND USE
This test method indicates the ability of the emulsion to withstand mild to moderately severe winter conditions of use and storage. Generally this significance would be limited to conditions where the emulsion reaches a minimum temperature of −18°C (0°F).
SCOPE
1.1 This test method covers the indication of the stability of water-in-oil emulsions when subjected to temperature cycling changes between ambient temperature and -18C (0F).
1.2 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.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.

General Information

• Status: Historical
• Publication Date: 30-Apr-2005
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants

Relations

• Replaces: ASTM D3709-89(1999) - Standard Test Method for Stability of Water-in-Oil Emulsions Under Low to Ambient Temperature Cycling Conditions
• Effective Date: 01-May-2005
• Replaced By: ASTM D3709-89(2010) - Standard Test Method for Stability of Water-in-Oil Emulsions Under Low to Ambient Temperature Cycling Conditions (Withdrawn 2016)
• Effective Date: 01-Oct-2010
• Referred By: ASTM D6361/D6361M-98(2020) - Standard Guide for Selecting Cleaning Agents and Processes
• Effective Date: 01-May-2005

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation:D3709–89(Reapproved 2005)
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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Warning notes were editorially moved into text in May 2005.
1. Scope separated.Inaddition,watercontentsofthesampleatspecified
levels in the upper and lower layers of the sample are also
1.1 This test method covers the indication of the stability of
obtained.
water-in-oil emulsions when subjected to temperature cycling
changes between ambient temperature and –18°C (0°F).
4. Significance and Use
1.2 This standard does not purport to address all of the
4.1 This test method indicates the ability of the emulsion to
safety concerns, if any, associated with its use. It is the
withstand mild to moderately severe winter conditions of use
responsibility of the user of this standard to establish appro-
and storage. Generally this significance would be limited to
priate safety and health practices and determine the applica-
conditionswheretheemulsionreachesaminimumtemperature
bility of regulatory limitations prior to use.
of−18°C (0°F).
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
5. Apparatus
only.
5.1 Cold Box—Athermostaticallycontrolledfreezerorcold
box capable of being maintained at−18 6 1.5°C (0 6 3°F).
2. Referenced Documents
5.2 Graduated Cylinder—A stoppered 100-mL glass cylin-
2.1 ASTM Standards:
der graduated in 1.0-mL increments. The stopper should have
D1744 TestMethodforWaterinLiquidPetroleumProducts
a vent groove to prevent vacuum or pressure build-up during
by Karl Fischer Reagent
the test.
3. Summary of Test Method 5.3 Pipet, 10-mL glass.
5.4 Microsyringe,0.05-mLglasswithafixedneedle,No.19
3.1 A 100-mL sample contained in a graduated 100-mL
gage, point style No. 3.
cylinderisplacedinacoolingboxat−18°C(0°F)for16hand
5.5 Glass Vials, approximately 30-mL size.
thenallowedtostandatroomtemperaturefor8h.Thiscycling
procedure is repeated to give a total of nine cycles, except that
6. Preparation of Sample
the fifth cycle is one of 64 h at−18°C (0°F), 8 h at room
6.1 To ensure uniformity of the sample, it should be mixed
temperature. At the completion of the cycling procedure the
thoroughly before removing the quantity required for the test.
sample is examined for the amount of free oil and free water
Vigorous hand shaking or mechanical mixing for 3 to 5 min is
recommended for litre-size containers or less.
This test method is under the jurisdiction of ASTM Committee D02 on
6.2 Special difficulties arise in mixing and withdrawing
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
representativesamplesfromlargecontainers.Thisisduetothe
D02.N0 on Hydraulic Fluids.
nature of water-in-oil emulsions that are two-phase systems as
Current edition approved May 1, 2005. Published May 2005. Originally
distinct from truly homogeneous systems. Vigorous mechani-
approved in 1978. Last previous edition approved in 1999 as D3709–89(1999).
DOI: 10.1520/D3709-89R05E01.
cal stirring for an extended period is the best means of
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
achieving homogeneity. However, for unstable emulsions that
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
havebeeninstorageforsometimethereisnosatisfactoryway
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. to obtain a representative sample.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
´1
D3709–89 (2005)
TABLE 1 Repeatability and Reproducibility For Type 1 Only
7. Procedure
Difference in %
7.1 After careful preparation of the sample to ensure homo-
Water Content
Free Oil, % Free Water, %
geneity (described in Section 6), transfer 100 mL to a gradu-
Upper Layer Versus
Lower Layer
ated 100-mL cylinder. Insert the vented stopper.
7.2 Place the cylinder in the cold box at−18 6 1.5°C (0 6
Repeatability 1 1 3
Reproducibility 2 2 3
3°F) for a period of 16 h.Withdraw the cylinder from the cold
box and allow to stand at room temperature, 21 6 3°C (70 6
5°F), for a period of 8 h.
7.3 Repeat the cycling procedure as in 7.2 for three more
9.1.1 Type I—Stable Emulsions (Procedures A and B):
cycles.
7.4 Replace the cylinder in the cold box for a period of 64 9.1.1.1 Precision—The precision of the method as deter-
h. Withdraw and allow to stand at room temperature for 8 h. mined by the statistical examination of interlaboratory test
7.5 Repeat the cycling procedure as in 7.2 for four more
results is as follows.
cycles, except that during the final cycle, the period at room
9.1.1.2 Repeatab
...