ASTM D6979-13
(Test Method)Standard Test Method for Polyurethane Raw Materials: Determination of Basicity in Polyols, Expressed as Percent Nitrogen
Standard Test Method for Polyurethane Raw Materials: Determination of Basicity in Polyols, Expressed as Percent Nitrogen
SIGNIFICANCE AND USE
5.1 This test method is suitable for quality control, as a specification test, and for research. The results are measures of batch-to-batch uniformity and are useful in estimating reactivity.
5.1.1 The percent nitrogen can be used to characterize a polyol or indicate amounts of certain components in a polyol blend.
5.1.2 It is permissible to also express the results in equivalents of base per gram of sample, if desired.
SCOPE
1.1 This test method measures the basic constituents in polyols that are soluble in glacial acetic acid and reactive with perchloric acid. Samples containing 0.3 – 10 % nitrogen have been evaluated by this method. This test method is applicable to polyether polyols and polyether polyol blends that are used in urethane reactions. (See Note 1.)
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.Note 1—This standard is equivalent to ISO 25761:08
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Designation: D6979 − 13
Standard Test Method for
Polyurethane Raw Materials: Determination of Basicity in
1
Polyols, Expressed as Percent Nitrogen
This standard is issued under the fixed designation D6979; 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:
3.2.1 percent nitrogen—the quantity of perchloric acid-
1.1 This test method measures the basic constituents in
titratable base, expressed as a weight percentage of nitrogen in
polyols that are soluble in glacial acetic acid and reactive with
a sample.
perchloric acid. Samples containing 0.3 – 10 % nitrogen have
been evaluated by this method. This test method is applicable
4. Summary of Test Method
to polyether polyols and polyether polyol blends that are used
in urethane reactions. (See Note 1.)
4.1 The sample is dissolved in glacial acetic acid. The
resulting single-phase solution is titrated at room temperature
1.2 The values stated in SI units are to be regarded as
to a potentiometric end point with a standardized solution of
standard. No other units of measurement are included in this
perchloric acid in acetic acid. Results are reported as percent
standard.
nitrogen.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.1 This test method is suitable for quality control, as a
bility of regulatory limitations prior to use.
specification test, and for research. The results are measures of
batch-to-batch uniformity and are useful in estimating reactiv-
NOTE 1—This standard is equivalent to ISO 25761:08
ity.
2. Referenced Documents
5.1.1 The percent nitrogen can be used to characterize a
2
2.1 ASTM Standards:
polyol or indicate amounts of certain components in a polyol
D883 Terminology Relating to Plastics
blend.
E180 Practice for Determining the Precision of ASTM
5.1.2 It is permissible to also express the results in equiva-
Methods for Analysis and Testing of Industrial and Spe-
lents of base per gram of sample, if desired.
3
cialty Chemicals (Withdrawn 2009)
E691 Practice for Conducting an Interlaboratory Study to
6. Apparatus
Determine the Precision of a Test Method
6.1 Potentiometric Automatic Titrator
3. Terminology
6.2 Autotitrator Buret with Dosing Device, 20-mL
3.1 Definitions—For definitions of terms used in this test
6.3 pH Glass Electrode and Reference Electrode or a
method see Terminology D883.
Combination Glass Electrode
1 6.4 Analytical Balances, capable of weighing to the nearest
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
0.01g and 0.0001 g
Plastics and Elastomers.
6.5 Magnetic Stirrer/Hotplate
Current edition approved Nov. 1, 2013. Published November 2013. Originally
approved in 2003. Last previous edition approved in 2008 as D6979 - 08. DOI:
10.1520/D6979-13.
7. Reagents and Materials
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contactASTM Customer Service at service@astm.org. ForAnnual Book ofASTM
7.1 Purity of Reagents—Use reagent-grade chemicals in all
Standards volume information, refer to the standard’s Document Summary page on
tests. Unless otherwise indicated, it is intended that all reagents
the ASTM website.
3 conform to the specifications of the Committee on Analytical
The last approved version of this historical standard is referenced on
www.astm.org. Reagents of the American Chemical Society where such
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6979 − 13
4
TABLE 1 Round-Robin Percent Nitrogen Data in Accordance with
specifications are available. It is permissible to use other
A
Practice E180
grades provided it is first ascertained that the reagent is of
B C D E F
Material Average S S r R df
r R
sufficiently high purity to permit its use without lessening the
A 0.317 0.0007 0.0018 0.0020 0.0050 5
accuracy of the determination.
B 2.51 0.0046 0.0053 0.0129 0.0148 5
C 5.86 0.0079 0.0139 0.0221 0.0392 5
7.2 Acetic Acid, Glacial
D 9.45 0.0220 0.0217 0.0616 0.0618 5
A
7.3 Acetic Anhydride
Values in units of percent nitrogen.
B
S = within-laboratory standard deviation of the replicates.
r
7.4 Perchloric Acid, (70 % nominal) C
S = between-laboratories standard deviation of the average.
R
D
r =
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6979 − 08 D6979 − 13
Standard Test Method for
Polyurethane Raw Materials: Determination of Basicity in
1
Polyols, Expressed as Percent Nitrogen
This standard is issued under the fixed designation D6979; 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
1.1 This test method measures the basic constituents in polyols that are soluble in glacial acetic acid and reactive with perchloric
acid. Samples containing 0.3 – 10 % nitrogen have been evaluated by this method. This test method is applicable to polyether
polyols and polyether polyol blends that are used in urethane reactions. (See Note 1.)
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
NOTE 1—This standard is equivalent to ISO 25761:08
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions—For definitions of terms used in this test method see Terminology D883.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 percent nitrogen—the quantity of perchloric acid-titratable base, expressed as a weight percentage of nitrogen in a sample.
4. Summary of Test Method
4.1 The sample is dissolved in glacial acetic acid. The resulting single-phase solution is titrated at room temperature to a
potentiometric end point with a standardized solution of perchloric acid in acetic acid. Results are reported as percent nitrogen.
5. Significance and Use
5.1 This test method is suitable for quality control, as a specification test, and for research. The results are measures of
batch-to-batch uniformity and may be are useful in estimating reactivity.
5.1.1 The percent nitrogen can be used to characterize a polyol or indicate amounts of certain components in a polyol blend.
5.1.2 It is permissible to also express the results in equivalents of base per gram of sample, if desired.
6. Apparatus
6.1 Potentiometric Automatic Titrator
6.2 Autotitrator Buret with Dosing Device, 20-mL
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics
and Elastomers.
Current edition approved Aug. 1, 2008Nov. 1, 2013. Published September 2008November 2013. Originally approved in 2003. Last previous edition approved in 20032008
as D6979 - 03.D6979 - 08. DOI: 10.1520/D6979-08.10.1520/D6979-13.
2
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.
3
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6979 − 13
6.3 pH Glass Electrode and Reference Electrode or a Combination Glass Electrode
6.4 Analytical Balances, capable of weighing to the nearest 0.01g and 0.0001 g
6.5 Magnetic Stirrer/Hotplate
7. Reagents and Materials
7.1 Purity of Reagents—Use reagent-grade chemicals in all tests. Unless otherwise indicated, it is intended that all reagents
conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
4
specifications are available. It is permissible to use other grades provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the determination.
7.2 Acetic Acid, Glacial
7.3 Acetic Anhydride
7.4 Perchloric Acid, (70 % nominal)
7.5 Perchloric acid in Acetic Acid (0.10 N)—Prepare 0.10 N perchloric acid in acetic acid. Fo
...
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