Standard Test Methods for Hydroxyethylcellulose

SIGNIFICANCE AND USE
The results of this test are used for calculating the total solids in the sample; and, by common usage, all materials volatile at this test temperature are designated as moisture.
Moisture analysis (along with sulfated ash) is a measure of the amount of active polymer in the material and must be considered when determining the amount of hydroxyethyl cellulose to use in various formulations.
SCOPE
1.1 These test methods cover the testing of hydroxyethylcellulose.
1.2 The test procedures appear in the following order: SectionsMoisture4-9Ash10-17 Viscosity18-24Density25-31
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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Publication Date
31-May-2007
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ASTM D2364-01(2007)e1 - Standard Test Methods for Hydroxyethylcellulose
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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´1
Designation: D2364 − 01 (Reapproved2007)
Standard Test Methods for
Hydroxyethylcellulose
This standard is issued under the fixed designation D2364; 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.
ε NOTE—Specification E 1 was replaced with Specification E 2251 in Section 2 and 20.5 in June 2007.
1. Scope Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, pro-
1.1 These test methods cover the testing of hydroxyethyl-
vided it is first ascertained that the reagent is of sufficiently
cellulose.
high purity to permit its use without lessening the accuracy of
1.2 The test procedures appear in the following order:
the determination.
Sections
3.2 Unless otherwise indicated, reference to water shall be
Moisture 4-9
Ash 10-17 understood to mean reagent water, conforming to Specification
Viscosity 18-24
D1193.
Density 25-31
1.3 This standard does not purport to address all of the
MOISTURE
safety concerns, if any, associated with its use. It is the
4. Scope
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4.1 Thistestmethodcoversthedeterminationofthevolatile
bility of regulatory limitations prior to use.
content of hydroxyethylcellulose.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 The results of this test are used for calculating the total
D1193 Specification for Reagent Water
solids in the sample; and, by common usage, all materials
D4794 Test Method for Determination of Ethoxyl or Hy-
volatile at this test temperature are designated as moisture.
droxyethoxyl Substitution in Cellulose Ether Products by
5.2 Moisture analysis (along with sulfated ash) is a measure
Gas Chromatography
of the amount of active polymer in the material and must be
E2251 Specification for Liquid-in-Glass ASTM Thermom-
considered when determining the amount of hydroxyethyl
eters with Low-Hazard Precision Liquids
cellulose to use in various formulations.
3. Purity of Reagents
6. Apparatus
3.1 Reagent grade chemicals shall be used in all tests.
6.1 Oven, gravity-convection, capable of maintaining a
Unless otherwise indicated, it is intended that all reagents shall
temperature of 105 6 3°C.
conform to the specifications of the Committee on Analytical
6.2 Weighing Bottles, low-form, 50 mm in inside diameter
by 30 mm in height, or equivalent.
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
6.3 Analytical Balance.
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
CurrenteditionapprovedJune1,2007.PublishedJuly2007.Originallyapproved
in 1965. Last previous edition approved in 2001 as D2364 – 01. DOI: 10.1520/ Reagent Chemicals, American Chemical Society Specifications, American
D2364-01R07E01. Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
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
´1
D2364 − 01 (2007)
7. Procedure 15.3 Place the dish in a 825°C muffle furnace for 1 h, or
longer if required, to burn all of the carbon.
7.1 Weigh5gofsampletothenearest0.001ginataredand
covered weighing bottle. 15.4 Remove the dish, allow to cool somewhat, place in a
desiccator, and cool to room temperature. Weigh the dish and
7.2 Place it in an oven at 105°C for 2 h with the cover
residue to the nearest 0.0001 g.
removed. Replace the cover, cool in a desiccator, and weigh.
16. Calculation
8. Calculation
16.1 Calculate the percent of ash (as sulfate), C, as follows:
8.1 Calculate the percent moisture, M, as follows:
C 5 ~A/B! 3100 (2)
M 5 ~A/B! 3100 (1)
where:
where:
A = ash, g, and
A = mass loss on heating, g, and
B = sample used, g.
B = sample used, g.
17. Precision and Bias
9. Precision and Bias
17.1 Statistical analysis of interlaboratory (reproducibility)
9.1 Statistical analysis of intralaboratory (repeatability) test
test results on samples containing 2 to 5 % ash (as sulfate)
results on samples containing from about 3.5 % moisture
indicates a precision of 60.3 % absolute at the 95 % level.
indicate a precision of 60.5 % absolute at the 95 % confidence
17.2 No statement on bias can be made as no suitable
level.
reference material is available as a standard.
9.2 No statement on bias can be made as no suitable
reference material is available as a standard.
VISCOSITY
ASH—AS SULFATE
18. Scope
18.1 This test method is an arbitrary method of determining
10. Scope
the viscosity of aqueous solutions of hydroxyethylcellulose in
10.1 This test method covers the determination of the
the viscosity range from 10 to 10 000 cP at 25°C.
residue on ignition of hydroxyethylcellulose after a specimen
18.2 The concentration to be used for the test shall be
has been treated with sulfuric acid.
agreed upon between the purchaser and the seller. It shall be
such that the viscosity of the solution will fall within the range
11. Summary of Test Method
of this test.
11.1 Aspecimen is moistened with sulfuric acid, the excess
18.3 The results for the viscosity of hydroxyethylcellulose
acid evaporated, the carbonaceous matter burned off, and the
by this test method will not necessarily check with results from
residue ignited in a muffle furnace, cooled, and weighed.
other types of instruments used for viscosity measurements.
12. Significance and Use
18.4 The determinations are run on a calculated dry basis;
12.1 Excessive ash can affect solution clarity and film that is, the amount of hydroxyethylcellulose required for the
properties. The ash (along with moisture) is a measure of the desired concentration on a dry basis is calculated from the
amount of active polymer in the material and must be consid- known moisture content.
eredwhendeterminingtheamountofhydroxyethylcelluloseto
19. Significance and Use
use in various formulations.
19.1 This test method is intended for referee purposes. The
13. Apparatus
Brookfield spindles and speeds given in Table 1 are recom-
mended for this purpose, but slight deviations from may
13.1 Dishes, platinum, 50 to 75-mL capacity.
occasionally be found convenient for individual application.
13.2 Muffle Furnace, maintained at 825 6 25°C.
19.2 This test method determines the relative ability of the
14. Reagents
polymertothickenaqueoussolutionsandisthereforerelatedto
the concentration required in various formulations to achieve
14.1 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
the desired finished product viscosity.
(H SO ).
2 4
15. Procedure
TABLE 1 Viscometer
...

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