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for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D1176 − 14

Standard Practice for

Sampling and Preparing Aqueous Solutions of Engine
Coolants or Antirusts for Testing Purposes1
This standard is issued under the fixed designation D1176; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope 3. Significance and Use

1.1 This practice covers information on sampling and pre- 3.1 This practice is used commonly by vehicle service or
paring solutions of engine coolants and antirusts (Notes 1 and laboratory personnel for sampling and preparing aqueous
2). solutions of engine coolants or antirust for further evaluation
1.2 The values stated in SI units are to be regarded as the and testing.
standard. The values given in parentheses are approximate 3.2 This practice shall be followed when sampling and
equivalents given for information only. preparing aqueous solutions of products for evaluation in
1.3 This standard does not purport to address all of the ASTM test methods.
safety concerns, if any, associated with its use. It is the 3.3 Care must be taken to ensure that a representative
responsibility of the user of this standard to establish appro- sample of product is taken.
priate safety and health practices and determine the applica- 3.4 This practice describes several different test methods.
bility of regulatory limitations prior to use. The methods to be followed should be agreed to by the supplier
NOTE 1—Antirust as referred to in this practice covers products and the customer.
intended for use in automotive/light-duty and heavy-duty applications in
which water is used as the cooling medium. 4. Sampling Concentrated Liquid Products
NOTE 2—Antirust products are available in liquid and solid form. Solids 4.1 When received, the material will preferably be in a
should be handled as outlined in Annex A1. sealed, marked container. Allow the container to stand at room
2. Referenced Documents temperature (not below 20°C) before attempting to obtain a
sample. The container and its contents shall be shaken well
2.1 ASTM Standards:2 before sampling (see Note 3). Any signs of solution separation
D1122 Test Method for Density or Relative Density of should be noted and appropriate samples obtained by using a
Engine Coolant Concentrates and Engine Coolants By The decanting or pipeting technique. Some samples that contain
Hydrometer multiple phases may require the use of a separatory funnel to
D1193 Specification for Reagent Water isolate a particular liquid layer or solids.
D5931 Test Method for Density and Relative Density of
NOTE 3—In the case of larger containers such as those with a nominal
Engine Coolant Concentrates and Aqueous Engine Cool- volume of 20 or 200 L (5 or 55 gal), the contents should be mixed
ants by Digital Density Meter thoroughly with a stirrer for at least 5 min to ensure a homogeneous
mixture. The stirrer should be capable of dispersing any separated solids
and supernatant phases without drawing air into the mixture.
1
This practice is under the jurisdiction of ASTM Committee D15 on Engine 4.2 Remove a representative sample by pipeting or siphon-
Coolants and Related Fluids and is the direct responsibility of Subcommittee
D15.06 on Glassware Performance Tests.
ing.
Current edition approved April 1, 2014. Published April 2014. Originally
approved in 1951. Last previous edition approved in 2008 as D1176 – 98(2008).
5. Separation of Multiphase Products
DOI: 10.1520/D1176-14.
2
5.1 If the product contains separated solids or liquids, place
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
a representative sample obtained as described in Section 4 in a
Standards volume information, refer to the standard’s Document Summary page on separatory funnel. Stopper the funnel and allow to stand for at
the ASTM website. least 16 h. Separate the various phases as follows:

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1
D1176 − 14
5.1.1 Remove settled liquids or solids, if present, by allow- 6.3 Volumetric Procedure (Volume %):
ing them to drain out together with a minimum amount of the 6.3.1 For many applications, sufficient accuracy can be
major liquid phase. obtained by measuring the sample in a graduated cylinder.
5.1.2 Then drain the major liquid phase into a suitable 6.3.1.1 Measure the required volume of engine coolant or
container, taking care not to include any supernatant liquid antirust into a graduated cylinder.
phase. 6.3.1.2 Add water of the type to be used for the test to just
5.1.3 Finally, drain the supernatant phase into a separate below the final volume. Mix the solution well. Add enough
container. water of the type to be used for the test to bring the contents of
5.1.4 If the solids will not drain out from the separatory the graduated cylinder to the final volume and mix well again.
funnel, siphon off the various liquid phases in sequence from The test concentration shall be expressed as the ratio of the
the top of the funnel. initial volume of the product to the final volume of the mixture
5.1.5 If the solid does not separate from the liquid phase but of the product and water, both measured at 20°C.
remains in suspension, separate by passing a representative 6.3.2 More accurate concentrations can be prepared by the
sample of the product through an appropriate filter paper, using following procedure:
suction, and transfer the liquid to a storage container. 6.3.2.1 Suspend the sample in a constant temperature water
bath set at 20 6 0.1°C. Allow 15 to 30 min for the sample to
6. Preparation of Aqueous Solutions equilibrate to this temperature.
6.1 Concentration is generally expressed as the percentage 6.3.2.2 When the sample has reached bath temperature,
by volume of the product at a specified temperature, usually transfer the required volume by pipet (see Note 5) to a clean,
20°C (68°F). dry volumetric flask calibrated at 20 6 0.1°C.
6.2 Gravimetric Procedure (Weight/Volume %): NOTE 5—The pipet should be calibrated using the test solution at 20 6
0.1°C.
6.2.1 Determine the relative density of the product at
20/20°C (68/68°F) to the nearest 0.0005 in accordance with 6.3.2.3 Bring the level in the flask almost to the graduated
Test Method D1122 or D5931. mark with the type water to be used for the test. Mix the
6.2.2 Calculate the weight of the product required to give contents of the flask by inverting several times, taking care to
the volume at 20°C (68°F). avoid loss of solution through the stopper. Proceed as directed
in 6.2.4.
NOTE 4—Example—For a 30 % solution and a final volume of 100 mL,
a product that has a relative density of 1.0149 at 20/20°C (68/68°F) would 7. Preparation of Test Solutions that Contain Solids or
require that the following amount be weighed:
Liquid Mixtures, or Both, in the Sample to be Tested
0.30 3 100 3 ~ 1.0149 3 0.99715! 5 30.360 g of product (1) 7.1 It is difficult to handle and obtain accurate specific
where: gravity measurements on samples containing solids and sepa-
0.99715 = the density of water at 20°C (68°F). rated layers. They are generally handled best by following the
6.2.3 Weigh the sample in a clean, dry container on a recommendation outlined in 4.1.
balance at room temperature. The sample shall be weighed to 8. Treatment of Mixtures Resulting from Separation of
an accuracy of 60.02 %. Record the weight and transfer the Secondary Phases on Dilution of Product with Water
sample to a clean, dry volumetric flask. Care should be taken
to ensure that all of the sample is transferred from the weight 8.1 If a representative portion of the mixture is desired,
container by rinsing with Specification D1193, Type IV water proceed as directed in 4.1 before a portion is removed by
(or ASTM corrosive water, if required by the test). Fill to just pipeting or siphoning. Stirring should be continued during
below the mark. removal of the sample.
6.2.4 Mix the contents of the volumetric flask and bring to 8.2 If secondary phases are to be separated, proceed as
20°C (68°F) by placing the flask in a constant temperature bath directed in 5.1.
set at 20 6 0.1°C. Adjust the volume to the mark using the
specified water when the contents have had a chance to come 9. Keywords
to temperature. Transfer the solution to the test vessel or 9.1 antirust; aqueous solutions; engine coolant; gravimetric
storage container. procedure; sampling; solutions; volumetric procedure

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D1176 − 14
ANNEX

(Mandatory Information)

A1. HANDLING SOLID ANTIRUSTS

A1.1 Antirusts supplied as powder or granules shall be A1.2 Dried samples shall be weighed without delay to an
sampled by taking portions from various points of the con- accuracy of 60.02 %, placed in a volumetric flask, and diluted
tainer. In the case of solids or caked material, the entire to the specified concentration with whatever water is required
package shall be broken up, mixed thoroughly, and quartered, for the given test according to the procedure for a liquid
if necessary. The sample shall be dried at 100°C to a constant product.
weight and stored in a desiccator until used. Samples shall not
be taken from those portions of the inhibitor in which caking
has been caused by absorption of moisture and carbon dioxide
through the container.

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