This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

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

Designation: D4669 − 18

Standard Test Method for

Polyurethane Raw Materials: Determination of Specific
Gravity of Polyols 1
This standard is issued under the fixed designation D4669; 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.

1. Scope* 3.2 Definitions of Terms Specific to This Standard:

1.1 These test methods measure the specific gravity of 3.2.1 specific gravity—the ratio of the weight in air of a
polyols. Test Method A measures the specific gravity of polyols given volume of the material at a stated temperature to the
using a pycnometer and Test Method B lists a reference for weight in air of an equal volume of water at a stated
measuring the specific gravity of liquids using a density meter temperature. It shall be expressed as specific gravity, 25/25°C,
that is applicable to polyols (see Note 1). indicating that the sample and reference water were both
measured at 25°C.
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 appro- 4. Significance and Use
priate safety, health, and environmental practices and deter- 4.1 These test methods are suitable for quality control,
mine the applicability of regulatory limitations prior to use. specification testing, and research. The specific gravity is
NOTE 1—There is no known ISO equivalent to this standard. necessary when converting kinematic viscosity to absolute
viscosity.
1.3 This international standard was developed in accor-
dance with internationally recognized principles on standard-
TEST METHOD A—SPECIFIC GRAVITY USING A
ization established in the Decision on Principles for the
PYCNOMETER
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 5. Apparatus
5.1 Pycnometer, of 25 or 50-mL capacity, conical shape with
2. Referenced Documents
a capillary side arm overflow tube complete with a standard-
2.1 ASTM Standards:2 taper 5⁄12 ground-glass joint to receive a ground-glass vented
D883 Terminology Relating to Plastics cap. A thermometer with a scale graduated from 12 to 38°C in
D4052 Test Method for Density, Relative Density, and API 0.2-degree divisions joins the neck of the flask with a standard-
Gravity of Liquids by Digital Density Meter taper 10⁄18 ground-glass joint. The thermometer contained in the
E2251 Specification for Liquid-in-Glass ASTM Thermom- pycnometer shall be calibrated in accordance with Specifica-
eters with Low-Hazard Precision Liquids tion E2251.
E202 Test Methods for Analysis of Ethylene Glycols and
Propylene Glycols 5.2 Water Bath, capable of maintaining a temperature of
25.0 6 0.05°C during the test.
3. Terminology
5.3 Thermometer, an ASTM Low Softening Point Ther-
3.1 Definitions—For definitions of terms used in these test mometer having a range from -2 to +80°C and conforming to
methods see Terminology D883. the requirements for Thermometer S15C as prescribed in
Specification E2251.
1
These test methods are under the jurisdiction of ASTM Committee D20 on
Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular 5.4 Analytical Balance, sensitive to 0.1 mg.
Materials - Plastics and Elastomers. It was recommended to ASTM by the Center for
the Polyurethane Industry of the American Chemistry Council.
Current edition approved April 1, 2018. Published April 2018. Originally
6. Reagents
approved in 1987. Last previous edition approved in 2013 as D4669 – 07(2013)ɛ1.
DOI: 10.1520/D4669-18.
6.1 Chromic Acid Cleaning Solution—Prepare a saturated
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or solution of chromic acid (CrO3) in concentrated sulfuric acid
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM (H2SO4, sp gr 1.84).
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.2 Acetone, reagent grade

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D4669 − 18
7. Sampling 10. Precision and Bias
7.1 High molecular weight polyester and polyether polyols 10.1 Attempts to develop a precision and bias statement for
contain molecules covering an appreciable range of molecular this test method have not been successful. Data on precision
weights. These have a tendency to fractionate during solidifi- and bias cannot be given for this reason. Because this test
cation. Unless the material is a finely ground solid it is method does not contain a round robin-based numerical
necessary to melt (using no higher temperature than necessary) precision and bias statement, it shall not be used as a referee
and mix the polyol well before removing a sample for analysis. test method in case of dispute. It is recommended that anyone
Since many polyols are hygroscopic, take care to provide wishing to participate in the development of precision and bias
minimum exposure to atmospheric moisture during the sam- data should contact the Chairman, Subcommittee D20.22
pling. (Section D20.22.01), ASTM 100 Barr Harbor Drive, West
Conshohocken, PA 19428-2959.
8. Procedure
10.2 Test Methods E202 is similar and does include preci-
8.1 Clean the pycnometer by filling it with a chromic acid sion data. Precision statements from Test Methods E202 are
cleaning solution. Allow it to stand for a few hours, empty, and restated below as an estimate of the precision for this test
rinse well with distilled water. method.
8.2 Fill the pycnometer with freshly boiled distilled water 10.2.1 Repeatability—Precision under repeatability condi-
cooled to 23 6 1°C, and set the pycnometer thermometer in tions.
place carefully, avoiding trapping of air. Place the pycnometer 10.2.2 Reproducibility—Precision under reproducibility
in the water bath that has been maintained at 25.0 6 0.05°C for conditions.
at least 30 min and allow it to equilibrate to 25.0°C. Wipe the 10.2.3 Repeatability Limit—The value below which the
overflow from the side-arm capillary and cover with the vented absolute difference between two individual test results obtained
cap, remove from the bath, wipe dry, and weigh. under repeatability conditions may be expected to occur with a
8.3 Empty the pycnometer, rinse well with acetone and dry probability of approximately 0.95 (95 %). For E202, the
under vacuum for 15 min. Weigh the pycnometer and subtract maximum expected difference between two test results for the
the weight of the empty pycnometer from the weight when same material, obtained by the same operator using the same
filled with water in order to obtain the weight, W, of the equipment on the same day in the same laboratory due solely
contained water at 25°C in air. to the method is 0.0002 units.
10.2.4 Reproducibility Limit—The value below which the
8.4 The sample for test must be completely liquid. If the
absolute difference between two individual test results obtained
sample contains solid polyol, warm the entire sample in the
under reproducibility conditions may be expected to occur with
original container until it becomes liquid. Then cool the sample
a probability of approximately 0.95 (95 %). For E202, the
to 22 to 24°C and quickly fill the pycnometer with it, allowing
maximum expected difference between two test results for the
it minimal exposure to the atmosphere.
same material, obtained by different operators using different
8.5 Insert the thermometer carefully, avoiding trapping of equipment in different laboratories due solely to the method is
air. Place the pycnometer in the water bath that has been 0.0005 units.
maintained at 25.0 6 0.05°C for at least 30 min and allow it to
10.3 Bias—There are no recognized standards by which to
equilibrate to 25.0°C. Cover the side arm with the vented cap,
estimate the bias of this test method.
remove from the bath, wipe dry, and weigh. Subtract the
weight of the empty pycnometer from the weight when filled
with the sample in order to obtain the weight, S, of the TEST METHOD B—SPECIFIC GRAVITY USING A
contained sample at 25.0°C. DIGITAL DENSITY METER

9. Calculation 11. General

9.1 Calculate the specific gravity at 25/25°C as follows: 11.1 A general test method for specific gravity using a
digital density meter, which applies to polyols as well as other
S/W 5 Specific gravity, 25/25°C liquids is published in Test Method D4052.

where: 12. Keywords

S = sample used, g, and 12.1 density; polyols; polyurethane raw materials; specific
W = water in the pycnometer, g. gravity

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 D4669 − 18
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue
(D4669 – 07(2013)ɛ1) that may impact the use of this standard. (April 1, 2018)

(1) Subsection 1.1: Added fuller description of scope. (3) Section 10: Changed precision and bias statement to
(2) Subsection 8.2: Restated tolerance for consistency. comply with D4968–17.

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