ASTM D817-12
(Test Method)Standard Test Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate
Standard Test Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate
SIGNIFICANCE AND USE
7.1 Ash content gives an estimate of the inorganic content of cellulose ester samples. The presence of high levels of inorganic content (ash) can be detrimental to the melt stability and optical clarity of a cellulose ester in melt processing or act as a potential source of insolubles when the ester is used in solution.
SCOPE
1.1 These test methods cover procedures for the testing of cellulose acetate propionates and acetate butyrates. These esters may vary widely in composition and properties, so certain of the procedures can be used only in the ranges of composition where they are suitable.
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 The test procedures appear in the following sections:
Sections
Acetyl Propionyl or Butyryl Contents
28-37
Acetyl Content, Apparent
18-27
Acidity, Free
12-17
Ash
7-10
Color and Haze
77-81
Heat Stability
57-65
Hydroxyl Content
38-44
Hydroxyl Content, Primary
46-50
Intrinsic Viscosity
67-71
Moisture Content
5-6
Sulfur or Sulfate Content
51-56
Viscosity
74-75
Limiting Viscosity Number
67-71
1.4 This standard does not purport to address 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.
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Designation: D817 − 12
Standard Test Methods of Testing
Cellulose Acetate Propionate and Cellulose Acetate
1
Butyrate
This standard is issued under the fixed designation D817; 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.
1. Scope D2929Test Method for Sulfur Content of Cellulosic Mate-
rials by X-Ray Fluorescence
1.1 These test methods cover procedures for the testing of
D5897Test Method for Determination of Percent Hydroxyl
cellulose acetate propionates and acetate butyrates. These
on Cellulose Esters by Potentiometric Titration—
esters may vary widely in composition and properties, so
Alternative Method
certain of the procedures can be used only in the ranges of
composition where they are suitable.
3. Reagents
1.2 The values stated in SI units are to be regarded as the
3.1 Purity of Reagents—Reagent grade chemicals shall be
standard. The values given in parentheses are for information
used in all tests. Unless otherwise indicated, it is intended that
only.
all reagents shall conform to the specifications of the Commit-
1.3 The test procedures appear in the following sections:
tee onAnalytical Reagents of theAmerican Chemical Society,
3
where such specifications are available. Other grades may be
Sections
Acetyl Propionyl or Butyryl Contents 28–37
used, provided it is first ascertained that the reagent is of
Acetyl Content, Apparent 18–27
sufficiently high purity to permit its use without lessening the
Acidity, Free 12–17
accuracy of the determination.
Ash 7–10
Color and Haze 77–81
Heat Stability 57–65
4. Conditioning
Hydroxyl Content 38–44
Hydroxyl Content, Primary 46–50
4.1 Conditioning—Condition the test specimens at 23 6
Intrinsic Viscosity 67–71
2°C(73.4 63.6°F)and50 65%relativehumidityfornotless
Moisture Content 5-6
than 40 h prior to test in accordance with Procedure A of
Sulfur or Sulfate Content 51–56
Viscosity 74-75
Practice D618, for those tests where conditioning is required.
Limiting Viscosity Number 67–71
In cases of disagreement, the tolerances shall be 61°C
1.4 This standard does not purport to address the safety
(61.8°F) and 62% relative humidity.
concerns, if any, associated with its use. It is the responsibility
4.2 Test Conditions—Conduct tests in the Standard Labora-
of the user of this standard to establish appropriate safety and
tory Atmosphere of 23 6 2°C (73.4 6 3.6°F) and 50 65%
health practices and determine the applicability of regulatory
relative humidity, unless otherwise specified in the test meth-
limitations prior to use.
ods. In cases of disagreements, the tolerances shall be 61°C
(61.8°F) and 62% relative humidity.
2. Referenced Documents
2
2.1 ASTM Standards:
MOISTURE CONTENT
D618Practice for Conditioning Plastics for Testing
5. Procedure
D1343Test Method for Viscosity of Cellulose Derivatives
by Ball-Drop Method
5.1 Transfer about5gofthe sample to a tared, low,
wide-form weighing bottle and weigh to the nearest 0.001 g.
Dry in an oven for2hat105 6 3°C. Remove the bottle from
1
These test methods are under the jurisdiction of ASTM Committee D01 on
the oven, cover, cool in a desiccator, and weigh.
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved Nov. 1, 2012. Published January 2013. Originally
3
approved in 1944. Last previous edition approved in 2010 as D817–96(2010). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D0817-12. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D817 − 12
6. Calculation 12.3 Phenolphthalein Indicator Solution (1 g/100 mL)—
Dissolve 1gphenolphthalein in 100 mL of ethyl alco-
6.1 Calculate the percentage of moisture as follows:
hol (95%).
Moisture, % 5 A/B 3100 (1)
~ !
12.4 Sodium Hydroxide, Standard Solution (0.01 N)—
where:
Prepareandstandardizea0.01 Nsolutionofsodiumhydroxide
A = weight loss on heatin
...
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: D817 − 96 (Reapproved 2010) D817 − 12
Standard Test Methods of Testing
Cellulose Acetate Propionate and Cellulose Acetate
1
Butyrate
This standard is issued under the fixed designation D817; 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 These test methods cover procedures for the testing of cellulose acetate propionates and acetate butyrates. These esters may
vary widely in composition and properties, so certain of the procedures can be used only in the ranges of composition where they
are suitable.
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 The test procedures appear in the following sections:
Sections
Acetyl Propionyl or Butyryl Contents 28-37
Acetyl Content, Apparent 18-27
Acidity, Free 12-17
Ash 7-10
Color and Haze 77-81
Heat Stability 57-65
Hydroxyl Content 38-44
Hydroxyl Content, Primary 46-50
Intrinsic Viscosity 67-71
Moisture Content 5-6
Sulfur or Sulfate Content 51-56
Viscosity 74-75
Limiting Viscosity Number 67-71
1.4 This standard does not purport to address 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D618 Practice for Conditioning Plastics for Testing
D1343 Test Method for Viscosity of Cellulose Derivatives by Ball-Drop Method
D2929 Test Method for Sulfur Content of Cellulosic Materials by X-Ray Fluorescence
D5897 Test Method for Determination of Percent Hydroxyl on Cellulose Esters by Potentiometric Titration—Alternative
Method
2.2 ASTM Adjuncts:
3
Color and Haze Apparatus
3. Reagents
3.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
1
These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility of
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved June 1, 2010Nov. 1, 2012. Published July 2010January 2013. Originally approved in 1944. Last previous edition approved in 20042010 as
ε1
D817 – 96 (2004)(2010). . DOI: 10.1520/D0817-96R10.10.1520/D0817-12.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D817 − 12
3
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
4. Conditioning
4.1 Conditioning—Condition the test specimens at 23 6 2°C (73.4 6 3.6°F) and 50 6 5 % relative humidity for not less than
40 h prior to test in accordance with Procedure A of Practice D618, for those tests where conditioning is required. In cases of
disagreement, the tolerances shall be 61°C (61.8°F) and 62 % relative humidity.
4.2 Test Conditions—Conduct tests in the Standard Laboratory Atmosphere of 23 6 2°C (73.4 6 3.6°F) and 50 6 5 % relative
humidity, unless otherwise specified in the test methods. In cases of disagreements, the tolerances shall be 61°C (61.8°F) and
62 % relative humidity.
MOISTURE CONTENT
5. Procedure
5.1 Transfer about 5 g of the sample to a tared, low, wide-form weighing bottle and weigh to the nearest 0.001 g. Dry in an oven
for 2 h at 105 6 3°C. Remove the bottle from the oven, cover, cool in a desiccator, and weigh.
6. Calculation
6.1 Calculate the percentage of moisture as follows:
Moisture, %5 A/B 3100 (1)
~ !
where:
where:
A = weight loss on heating, g, and
B = sample used, g.
ASH
7. Significance and Use
7.1 Ash content gives an estimate of the inorganic content of cellulose ester samples. The presence of high level
...
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