ASTM D817 - 12 (2019)

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Designation: D817 −12 (Reapproved 2019)
Standard Test Methods of Testing
Cellulose Acetate Propionate and Cellulose Acetate
Butyrate
1
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 all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
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 Mate-
rials by X-Ray Fluorescence
D5897 Test Method for Determination of Percent Hydroxyl
on Cellulose Esters by Potentiometric Titration—
Alternative Method
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 Commit-
tee on Analytical Reagents of the American Chemical Society,
where such speciﬁcations are available.
3
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 63.6°F) and 50 65 % 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 Labora-
tory Atmosphere of 23 62°C (73.4 63.6°F) and 50 65%
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 Dec. 1, 2019. Published December 2019. Originally
approved in 1944. Last previous edition approved in 2012 as D817 – 12. DOI:
10.1520/D0817-12R19.
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
ACS Reagent Chemicals, Speciﬁcations and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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.
1
 

relative humidity, unless otherwise speciﬁed in the test meth-

ods. In cases of disagreements, the tolerances shall be 61°C

(61.8°F) and 62 % relative humidity.

MOISTURE CONTENT

5. Procedure

5.1 Transfer about5gofthesample to a tared, low,

wide-form weighing bottle and weigh to the nearest 0.001 g.

Dry in an oven for2hat10563°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:

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 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.

8. Procedure

8.1 Dry the sample for2hat10563°C and weigh 10 to 50

g, to the nearest 0.01 to 0.1 g, depending on its ash content and

the accuracy desired. Burn directly over a ﬂame in a 100-mL

tared platinum crucible that has been heated to constant weight

and weighed to the nearest 0.1 mg. Add the sample in portions

if more than 10 g is taken. The sample should burn gently and

the portions should be added as the ﬂame subsides. Continue

heating with a burner only as long as the residue burns with a

ﬂame. Transfer the crucible to a muffle furnace and heat at 550

to 600°C for 3 h, or longer if required, to burn all the carbon.

Allow the crucible to cool and then transfer it, while still warm,

to a desiccator. When the crucible has cooled to room

temperature, weigh accurately to the nearest 0.1 mg.

9. Calculation

9.1 Calculate the percentage of ash as follows:

Ash, % 5

A/B

3100 (2)

where:

A= ash, g, and

B= sample used, g.

10. Precision and Bias

10.1 No statement on bias can be made as no reference

material is available as a standard.

FREE ACIDITY

11. Signiﬁcance and Use

11.1 Free acidity is a measure of unesteriﬁed organic acid in

the ester. The presence of high levels of free acid is potentially

detrimental to melt processing of the ester and can impact the

odor of the ester.

12. Reagents

12.1 Acetone, neutral.

12.2 Methyl Red Indicator Solution (0.4 g/L)—Dissolve 0.1

g of methyl red in 3.72 mL of 0.1000 NNaOH solution and

dilute to 250 mL with water. Filter if necessary.

12.3 Phenolphthalein Indicator Solution (1 g/100 mL)—

Dissolve 1 g phenolphthalein in 100 mL of ethyl alco-

hol (95 %).

12.4 Sodium Hydroxide, Standard Solution (0.01 N)—

Prepare and standardize a 0.01 Nsolution of sodium hydroxide

(NaOH).

Test Method A—For Samples Containing Not More than

About 30 % Propionyl or Butyryl

13. Procedure

13.1 Shake5gofthesample, corrected for moisture content

if necessary, in a 250-mL Erlenmeyer ﬂask with 150 mL of

freshly boiled, cold water. Stopper the ﬂask and allow it to

stand for 3 h. Filter off the cellulose ester and wash it with

water. Titrate the combined ﬁltrate and washings with 0.01 N

NaOH solution, using phenolphthalein indicator solution.

13.2 Run a blank determination on the water, using the same

volume as was used in extracting the sample.

14. Calculation

14.1 Calculate the percentage of acidity as free acetic acid

as follows:

Free acetic acid, % 5

A2B

C30.06

3100 (3)

where:

A= NaOH solution used to titrate the sample, mL,

B= NaOH solution used to titrate the blank, mL,

C= normality of the NaOH solution, and

W= sample used, g.

Test Method B—For Samples Containing More than About

7 %Propionyl or Butyryl and Particularly Suitable for

Samples Containing More than 30 % Propionyl or Butyryl

15. Procedure

15.1 Dissolve 10.0 g of the sample, corrected for moisture

content if necessary, in 200 mL of neutral acetone plus 20 mL

of water. When completely dissolved, add 50 mL of water and

shake well to precipitate the ester in a ﬁnely divided form. Add

3 drops of methyl red indicator solution and titrate to a

lemon-yellow end point and 0.01 NNaOH solution.

15.2 Make a blank determination on the reagents.

D817 − 12 (2019)

16. Calculation

16.1 Calculate the free acid content as acetic acid as

directed in Section 14.

17. Precision and Bias

17.1 No statement on bias can be made as no reference

material is available as a standard.

APPARENT ACETYL CONTENT

18. Scope

18.1 The test methods described in the following Sections

20 to 26 cover the determination of the saponiﬁcation value of

the sample calculated as percentage of apparent acetyl, equiva-

lent weight 43. This value is required in the calculation of

acetyl and propionyl or butyryl contents in 36.1.

18.2 The test method used should be speciﬁed or agreed

upon. The choice depends on the propionyl or butyryl content

and the physical condition of the sample. Ordinarily, Test

Method A is recommended for samples having less than about

35 % propionyl or butyryl and Test Method B for samples

having more than that amount.

18.3 This international standard was developed in accor-

dance with internationally recognized principles on standard-

ization established in the Decision on Principles for the

Development of International Standards, Guides and Recom-

mendations issued by the World Trade Organization Technical

Barriers to Trade (TBT) Committee.

19. Signiﬁcance and Use

19.1 Apparent acetyl content is a measure of the saponiﬁ-

cation value of the ester. Apparent acetyl value is required in

the calculation of acetyl, propionyl, and butyryl content in

36.1.

Test Method A—For Samples Containing Less than About

35 % Propionyl or Butyryl

20. Apparatus

20.1 Weighing Bottle, glass-stoppered, 15-mL capacity,

25-mm diameter by 50 mm high.

20.2 Tray, copper or aluminum, approximately 137 mm

square, containing 25 compartments 25 mm square. Each

compartment shall have the correct dimensions to contain one

weighing bottle. The entire tray shall ﬁt inside a desiccator and

should have a basket-type handle to facilitate the introduction

and removal of the tray (convenient but not essential).

20.3 Buret, automatic zero, 35-mL, 25-mL bulb, stem

graduated from 25 to 35 mL in 0.05-mL increments; or pipet,

automatic zero, 30-mL for NaOH solution (40 g/L).

20.4 Buret, automatic zero, 15-mL, 10-mL bulb, stem

graduated from 10 to 15 mL in 0.05-mL increments, for 1 N

20.5 Buret, 5-mL, in 0.01 or 0.1-mL divisions, for back

titration with 0.1 NNaOH solution.

20.6 Magnetic Stirrer, for single ﬂask.

20.7 Magnetic Stirrer, capacity twelve or more ﬂasks.

20.8 Stirring Bars, stainless steel Type 416, length 50 mm,

diameter 5 to 6 mm or equivalent, dimensions not critical.

21. Reagents

21.1 Acetone—Add one 30-mL portion of 1.0 NNaOH

solution to a mixture of 150 mL acetone and 100 mL hot water,

allow to stand with frequent swirling for 30 min, and titrate

with 1.0 NH

. Add another 30-mL portion of 1.0 NNaOH

solution to 100 mL of hot water, allow to stand for 30 min, and

titrate as above. The difference between the two titrations shall

not exceed 0.05 mL.

21.2 Dimethyl Sulfoxide.

21.3 Pyridine.

21.4 Sodium Hydroxide Solution (40 g/L)—Dissolve 40 g of

sodium hydroxide (NaOH) in water and dilute to 1 L.

21.5 Sodium Hydroxide, Standard Solution (0.1 N)—

Prepare and standardize a 0.1 Nsolution of NaOH.

21.6 Sulfuric Acid Standard (1.0 N)—Prepare and standard-

ize a 1.0 Nsolution of sulfuric acid (H

21.7 Phenolphthalein Indicator Solution (1 g/100 mL)—

Dissolve1gofphenolphthalein in 100 mL of ethyl alcohol

(95 %).

22. Procedure

22.1 Dry the ground well-mixed sample in weighing bottle

for2hat10563°C and weigh 1.9 60.05 g of the dried

sample by difference to the nearest 1 mg into a 500-mL

Erlenmeyer ﬂask. Prepare a blank by drying approximately 3.8

g of potassium acid phthalate and weighing it by difference into

a ﬂask as described above. Carry the blank through the entire

procedure.

NOTE 1—Potassium acid phthalate is used so that the concentration of

the NaOH in contact with the solvent in the blank will be approximately

the same as that in contact with the sample and so that the titration of the

blank will be approximately the same as the titration of the sample, thus

avoiding errors caused by using a different buret for the titration of the

blank and the sample or by reﬁlling the 15-mL buret. If desired, however,

the potassium acid phthalate may be omitted.

22.2 For acetone-soluble sample, put the sample into solu-

tion as follows: Add 150 mL of acetone and 5 to 10 mL of

water and swirl to mix. Stopper the ﬂask and allow it to stand

with occasional swirling until solution is complete. Solution

may be hastened by magnetic stirring or by any suitable

mechanical shaking that will provide a gentle rocking type of

agitation to avoid splashing the solution on the stopper. It is

essential that complete solution be effected.

22.3 For acetone-insoluble samples of low propionyl or

butyryl content, dissolve the sample by either of the following

two methods:

22.3.1 Gently rotate the ﬂask by hand to distribute and

spread the sample in a thin layer over the bottom of the ﬂask.

Add 70 mL of acetone to the ﬂask and swirl gently until the

sample particles are completely wetted and evenly dispersed.

Stopper the ﬂask and allow it to stand undisturbed for 10 min.

Carefully add 30 mL of dimethyl sulfoxide from a graduate to

D817 − 12 (2019)

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摘要：

ASTM D817 - 12 (2019) 是美国材料与试验协会发布的一项标准规范，主要针对纤维素醋酸酯塑料中增塑剂含量的测定方法。该标准最初于2012年批准，并在2019年进行了重新确认，以确保其技术内容与当前行业实践保持一致。标准详细规定了通过溶剂萃取、气相色谱分析等技术手段，定量测定醋酸纤维素塑料中常用增塑剂（如邻苯二甲酸酯类）的步骤与要求。适用于质量控制、材料认证及研究开发等领域，尤其对塑料制品制造商、检测实验室以及相关法规合规部门具有重要参考价值。遵循ASTM D817 - 12 (2

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