ASTM D5897-13
(Test Method)Standard Test Method for Determination of Percent Hydroxyl on Cellulose Esters by Potentiometric Titration—Alternative Method
Standard Test Method for Determination of Percent Hydroxyl on Cellulose Esters by Potentiometric Titration—Alternative Method
SIGNIFICANCE AND USE
4.1 This test method provides a simpler means for the determination of the hydroxyl content of cellulose esters than the preparation and measurement of the carbanilate derivative described in Test Methods D817 and D871.
4.2 The hydroxyl content is an important indicator of solubility and reactivity.
SCOPE
1.1 This test method covers a procedure for determining the percent hydroxyl on cellulose esters by potentiometric titration. The typical range of percent hydroxyl measured is 0.7 to 10.0 %.
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.
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Designation: D5897 − 13
Standard Test Method for
Determination of Percent Hydroxyl on Cellulose Esters by
1
Potentiometric Titration—Alternative Method
This standard is issued under the fixed designation D5897; 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 endpoint, and calculates the percent hydroxyl on the cellulose
ester based on a blank determination.
1.1 This test method covers a procedure for determining the
percenthydroxyloncelluloseestersbypotentiometrictitration.
4. Significance and Use
The typical range of percent hydroxyl measured is 0.7 to
4.1 This test method provides a simpler means for the
10.0 %.
determination of the hydroxyl content of cellulose esters than
1.2 The values stated in SI units are to be regarded as
the preparation and measurement of the carbanilate derivative
standard. No other units of measurement are included in this
described in Test Methods D817 and D871.
standard.
4.2 The hydroxyl content is an important indicator of
1.3 This standard does not purport to address all of the
solubility and reactivity.
safety concerns, if any, associated with its use. It is the
5. Interferences
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.1 Undissolved ester may accumulate on the sides of the
bility of regulatory limitations prior to use. flask and on top of the stirring-star during dissolution, leading
to low results. Gently swirling the solution during titration can
2. Referenced Documents
reduce this problem.
2
2.1 ASTM Standards:
5.2 The ground glass joints of the flask and the air con-
D817 Test Methods of Testing CelluloseAcetate Propionate
denser must always be rinsed into the flask with hydrolyzing
and Cellulose Acetate Butyrate
solutionatthepointofhydrolysisandbeforetitration.Thiswill
D871 Test Methods of Testing Cellulose Acetate
prevent erroneous results from material that may have refluxed
into the joint.
3. Summary of Test Method
6. Apparatus
3.1 The cellulose ester is dissolved in pyridine and the
hydroxyl sites on the cellulose ester are acetylated with acetic 6.1 Titrator, equipped with Glass Electrode.
anhydride in the presence of basic catalyst, 1-methylimidazole.
6.2 Heating/Stirring Module, six-place.
The excess acetic anhydride is hydrolyzed and the resulting
6.3 Heating/Stirring Block, cut from polished-finish alumi-
acetic acid is titrated with sodium hydroxide. An automatic
num block to fit stirrer in 6.2 (see Fig. 1 for dimensions).
titrator dispenses the titrant, potentiometrically determines the
6.4 Stirrer, six place.
1 6.5 Magnetic Stirrers, size 25 mm and 50 mm.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
6.6 Stirring Bar.
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved June 1, 2013. Published June 2013. Originally 6.7 Flask and Air Condenser, (see Fig. 2 for dimensions).
approved in 1996. Last previous edition approved in 2007 as D5897 – 96 (2007).
6.8 Bottle-Top Dispensers, capable of dispensing 20 mL, 35
DOI: 10.1520/D5897-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or mL, and 50 mL, or equivalent.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.9 Analytical Balance, capable of weighing 250 g to the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. fourth decimal place.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5897 − 13
FIG. 1 Heating/Stirring Block Dimensions
6.10 Analytical Balance, capable of weighing 1000 g to the
second decimal place.
7. Reagents and Materials
3
7.1 Purity of Reagents—American Chemical Society re-
agent grade chemicals shall be used throughout this test unless
otherwise indicated.
7.2 Pyridine.
7.3 Acetic Anhydride.
7.4 Acetylating Solution—115 6 0.50 g of acetic anhydride
per litre of pyridine. The container needs to be equipped with
20-mL buret. The shelf-life of this solution is 5 days.
7.5 Dimethylformamide.
7.6 Deionized Water, purified to 18.3 MΩ resistance.
7.7 Hydrolyzing Solution—Mix 600 mL
dimethylformamide, 300 mL pyridine, and 100 mL water in a
1-L bottle equipped with a bottle top dispenser capable of
dosing 35 mL. Stir for at least 10 min prior to use. The
shelf-life of this solution is 1 month.
7.8 1-Methylimidazole.
7.9 Sucrose.
7.10 Acetone
...
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: D5897 − 96 (Reapproved 2007) D5897 − 13
Standard Test Method for
Determination of Percent Hydroxyl on Cellulose Esters by
1
Potentiometric Titration—Alternative Method
This standard is issued under the fixed designation D5897; 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 covers a procedure for determining the percent hydroxyl on cellulose esters by potentiometric titration. The
typical range of percent hydroxyl measured is 0.7 to 10.0 %.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D817 Test Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate
D871 Test Methods of Testing Cellulose Acetate
3. Summary of Test Method
3.1 The cellulose ester is dissolved in pyridine and the hydroxyl sites on the cellulose ester are acetylated with acetic anhydride
in the presence of basic catalyst, 1-methylimidazole. The excess acetic anhydride is hydrolyzed and the resulting acetic acid is
titrated with sodium hydroxide. An automatic titrator dispenses the titrant, potentiometrically determines the endpoint, and
calculates the percent hydroxyl on the cellulose ester based on a blank determination.
4. Significance and Use
4.1 This test method provides a simpler means for the determination of the hydroxyl content of cellulose esters than the
preparation and measurement of the carbanilate derivative described in Test Methods D817 and D871.
4.2 The hydroxyl content is an important indicator of solubility and reactivity.
5. Interferences
5.1 Undissolved ester may accumulate on the sides of the flask and on top of the stirring-star during dissolution, leading to low
results. Gently swirling the solution during titration can reduce this problem.
5.2 The ground glass joints of the flask and the air condenser must always be rinsed into the flask with hydrolyzing solution
at the point of hydrolysis and before titration. This will prevent erroneous results from material that may have refluxed into the
joint.
6. Apparatus
6.1 Titrator, equipped with Glass Electrode,Electrode. or equivalent.
6.2 Heating/Stirring Module, six-place.
6.3 Heating/Stirring Block, cut from polished-finish aluminum block to fit stirrer in 7.26.2 (see Fig. 1 for dimensions).
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved June 1, 2007June 1, 2013. Published August 2007June 2013. Originally approved in 1996. Last previous edition approved in 20012007 as D5897
– 96 (2001).96 (2007). DOI: 10.1520/D5897-96R07.10.1520/D5897-13.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5897 − 13
FIG. 1 Heating/Stirring Block Dimensions
6.4 Stirrer, six place.
6.5 Magnetic Stirrers, size 25 mm and 50 mm.
6.6 Stirring Bar.
6.7 Flask and Air Condenser, (see Fig. 2 for dimensions).
6.8 Bottle-Top Dispensers, capable of dispensing 20 mL, 35 mL, and 50 mL, or equivalent.
6.9 Analytical Balance, capable of weighing 250 g to the fourth decimal place.
6.10 Analytical Balance, capable of weighing 1000 g to the second decimal place.
7. Reagents and Materials
3
7.1 Purity of Reagents—American Chemical Society reagent grade chemicals shall be used throughout this test unless
otherwise indicated.
7.2 Pyridine.
7.3 Acetic Anhydride.
7.4 Acetylating Solution—115 6 0.50 g of acetic anhydride per litre of pyridine. The container needs to be equipped with 20-mL
buret. The shelf-life
...
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