ASTM D4094-00

Standard Test Method for Acid Content of Ethylene-Acrylic Acid Copolymers

SIGNIFICANCE AND USE
EAA copolymers possess unusual chemical and physical properties because they contain free acid groups. Since polymer performance in end-use applications is a function of the amount of copolymerized acrylic acid, it is important that acid contents be determined quantitatively by a suitable method, such as that described herein.
SCOPE
1.1 This test method covers the determination of the acid content of ethylene-acrylic acid (EAA) copolymers containing 2.5 to 25 weight % of acrylic acid.
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.
Note 1--There is no similar or equivalent ISO standard

General Information

• Status: Historical
• Publication Date: 09-Jul-2000
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaced By: ASTM D4094-07 - Standard Test Method for Acid Content of Ethylene-Acrylic Acid Copolymers (Withdrawn 2015)
• Effective Date: 01-Nov-2007

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:D4094–00
Standard Test Method for
Acid Content of Ethylene-Acrylic Acid Copolymers
This standard is issued under the fixed designation D 4094; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope* 5. Significance and Use
1.1 This test method covers the determination of the acid 5.1 EAAcopolymerspossessunusualchemicalandphysical
content of ethylene-acrylic acid (EAA) copolymers containing properties because they contain free acid groups. Since poly-
2.5 to 25 weight % of acrylic acid. mer performance in end-use applications is a function of the
1.2 The values stated in SI units are to be regarded as the amount of copolymerized acrylic acid, it is important that acid
standard. The values given in parenthesis are for information contents be determined quantitatively by a suitable method,
only. such as that described herein.
1.3 This standard does not purport to address all of the
6. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 6.1 Balance, analytical, accurate to 0.0001 g.
6.2 Buret, 25-mL, 0.1-mL subdivisions, Class A, polytet-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazards rafluoroethylene stopcock.
6.3 Flask,Erlenmeyer,250-mL,femalestandard-taperjoint,
statements are given in Section 8.
with condenser, reflux, matching male standard-taper joint.
NOTE 1—There is no similar or equivalent ISO standard.
6.4 Stirrer/Hotplate, magnetic.
6.5 Stirrer, magnetic.
2. Referenced Documents
6.6 Stirring Bar, magnetic, 40 mm (1.5 in.) long,
2.1 ASTM Standards:
2 polytetrafluoroethylene-encased.
D 1898 Practice for Sampling of Plastics
E 177 Practice for Use of the Terms Precision and Bias in
7. Reagents and Materials
ASTM Test Methods
7.1 Xylene, reagent-grade.
E 691 Practice for Conducting an Interlaboratory Study to
7.2 n-Butanol, reagent-grade.
Determine the Precision of a Test Method
7.3 Mixed Solvent—Mix 3 volumes of xylene with 1 vol-
IEEE/ASTM SI–10 Standard for Use of the International
ume of n-butanol.
System of Units (SI): The Modern Metric System
7.4 Tetrabutylammonium Hydroxide (TBAH), solution in
methanol or benzene, in 1 M concentration.
3. Terminology
7.5 Standard Base (0.1 N)—Mix 1 volume of 1 M TBAH
3.1 Units and symbols used in this test method are those
solution with 9 volumes of mixed solvent.
recommended in IEEE/ASTM SI–10. Additional acronyms
7.6 Benzoic Acid, primary standard.
unique to this test method are defined in the text.
7.7 Thymol Blue (TB) Indicator (Formula Weight of
466.58)—Prepare 0.5 % solution by weighing 0.125 g of
4. Summary of Test Method
reagent-grade TB (acid form) into a small beaker, adding 25
4.1 In this test method, a weighed specimen is dissolved in
mLof mixed solvent, and adding 0.268 milliequivalents of 0.1
a suitable hot solvent and titrated while hot with standard base
N base to form a clear, red-orange solution. Transfer to a glass
to a visual equivalence point.
dropping bottle.
This test method is under the jurisdiction ofASTM Committee D20 on Plastics 8. Hazards
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
8.1 Solvents and titrants are malodorous and flammable and
(Section D20.70.11).
can cause burns to skin, eyes, and lungs.Wear proper body and
Current edition approved Nov. 10, 2000. Published February 2001. Originally
published as D 4094 – 82. Last previous edition D 4094 – 97.
eye protection when handling these materials and conduct all
Discontinued. See 1998 Annual Book of ASTM Standards , Vol 08.01.
operations in a fume hood from which all possible sources of
Annual Book of ASTM Standards, Vol 14.02.
4 ignition have been removed.
Annual Book of ASTM Standards, Vol 14.04.
*A Summary of Changes section appears at the end of this standard.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
D4094–00
TABLE 1 Acrylic Acid Content
9. Sampling
Materials Average S S rR
r R
9.1 Analyze pelletized samples in the form as received.
6.6% 6.6833 0.0370 0.0769 0.1035 0.2153
Analyze samples in duplicate.
9.5% 9.4467 0.1252 0.1477 0.3505 0.4136
9.2 If the intent is to determine within–lot uniformity or to
20.1% 20.2344 0.1044 0.3083 0.2923 0.8632
determine the conformity of a lot to specification limits for
20.2% 20.4150 0.1772 0.3549 0.4961 0.9937
average acid content, sample the lot in accordance with
principles outlined in Practice D 1898.
flask to a condenser and begin stirring and rapid heating.When
10. Standardization
boiling begins, reduce the heat to produce a steady moderate
10.1 Weigh out 0.2 to 0.3 g of benzoic acid and record its
stream of reflux from the condenser tip. Reflux until specimen
weight to 0.0001 g.Transfer to a flask containing a stirring bar,
is dissolved (for 30 min, or longer if necessary).
add 100 mL of mixed solvent, and stir at room temperature
12.3 Stop stirring and heating. Transfer flask containing
until dissolved.
dissolved specimen to an unheated stirrer, begin stirring, add 6
10.2 Add 6 drops of TB indicator and titrate with 0.1 N drops ofTB indicator, and titrate while hot from a yellow color
TBAH solution to the yellow-to-green-
...