ASTM D2364-96
(Test Method)Standard Test Methods for Hydroxyethylcellulose
Standard Test Methods for Hydroxyethylcellulose
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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Designation: D 2364 – 96
Standard Test Methods for
Hydroxyethylcellulose
This standard is issued under the fixed designation D 2364; 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 vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
1.1 These test methods cover the testing of hydroxyethyl-
the determination.
cellulose.
3.2 Unless otherwise indicated, reference to water shall be
1.2 The test procedures appear in the following order:
understood to mean reagent water, conforming to Specification
Sections
D 1193.
Moisture 4-9
Ash 10-17
Viscosity 18-24
MOISTURE
Density 25-31
Molar Substitution 32-42
4. Scope
1.3 This standard does not purport to address all of the
4.1 This test method covers the determination of the volatile
safety concerns, if any, associated with its use. It is the
content of hydroxyethylcellulose.
responsibility of the user of this standard to establish appro-
5. Significance and Use
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5.1 The results of this test are used for calculating the total
solids in the sample; and, by common usage, all materials
2. Referenced Documents
volatile at this test temperature are designated as moisture.
2.1 ASTM Standards:
5.2 Moisture analysis (along with sulfated ash) is a measure
D 1193 Specification for Reagent Water
of the amount of active polymer in the material and must be
D 1347 Test Methods for Methylcellulose
considered when determining the amount of hydroxyethyl
D 1695 Terminology of Cellulose and Cellulose Deriva-
cellulose to use in various formulations.
tives
6. Apparatus
D 2363 Test Methods for Hydroxypropyl Methylcellulose
D 4794 Test Method for Determination of Ethoxyl or Hy-
6.1 Oven, gravity-convection, capable of maintaining a
droxyethoxyl Substitution in Cellulose Ether Products by
temperature of 105 6 3°C.
Gas Chromatography
6.2 Weighing Bottles, low-form, 50 mm in inside diameter
E 1 Specification for ASTM Thermometers
by 30 mm in height, or equivalent.
6.3 Analytical Balance.
3. Purity of Reagents
7. Procedure
3.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
7.1 Weigh5gof sample to the nearest 0.001 g in a tared and
conform to the specifications of the Committee on Analytical
covered weighing bottle.
Reagents of the American Chemical Society, where such
7.2 Place it in an oven at 105°C for 2 h with the cover
specifications are available. Other grades may be used, pro-
removed. Replace the cover, cool in a desiccator, and weigh.
8. Calculation
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
8.1 Calculate the percent moisture, M, as follows:
and Related Coatings, Materials, and Applications and are the direct responsibility
of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
M 5 ~A/B! 3 100 (1)
Current edition approved Feb. 10, 1996. Published April 1996. Originally
published as D 2364 – 65 T. Last previous edition D 2364 – 89.
2 where:
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 06.03. A = mass loss on heating, g, and
Annual Book of ASTM Standards, Vol 14.03.
B = sample used, g.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
9. Precision and Bias
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia 9.1 Statistical analysis of intralaboratory (repeatability) test
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
results on samples containing from about 3.5 % moisture
MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 2364
indicate a precision of 60.5 % absolute at the 95 % confidence VISCOSITY
level.
18. Scope
9.2 No statement on bias can be made as no suitable
18.1 This test method is an arbitrary method of determining
reference material is available as a standard.
the viscosity of aqueous solutions of hydroxyethylcellulose in
ASH—AS SULFATE
the viscosity range from 10 to 10 000 cP at 25°C.
18.2 The concentration to be used for the test shall be
10. Scope
agreed upon between the purchaser and the seller. It shall be
10.1 This test method covers the determination of the
such that the viscosity of the solution will fall within the range
residue on ignition of hydroxyethylcellulose after a specimen
of this test.
has been treated with sulfuric acid.
18.3 The results for the viscosity of hydroxyethylcellulose
by this test method will not necessarily check with results from
11. Summary of Test Method
other types of instruments used for viscosity measurements.
11.1 A specimen is moistened with sulfuric acid, the excess
18.4 The determinations are run on a calculated dry basis;
acid evaporated, the carbonaceous matter burned off, and the
that is, the amount of hydroxyethylcellulose required for the
residue ignited in a muffle furnace, cooled, and weighed.
desired concentration on a dry basis is calculated from the
known moisture content.
12. Significance and Use
19. Significance and Use
12.1 Excessive ash can affect solution clarity and film
properties. The ash (along with moisture) is a measure of the
19.1 This test method is intended for referee purposes. The
amount of active polymer in the material and must be consid-
Brookfield spindles and speeds given in Table 1 are recom-
ered when determining the amount of hydroxyethyl cellulose to
mended for this purpose, but slight deviations from Table 1
use in various formulations.
may occasionally be found convenient for individual applica-
tion.
13. Apparatus
19.2 This test method determines the relative ability of the
13.1 Dishes, platinum, 50 to 75-mL capacity.
polymer to thicken aqueous solutions and is therefore related to
13.2 Muffle Furnace, maintained at 825 6 25°C.
the concentration required in various formulations to achieve
the desired finished product viscosity.
14. Reagents
20. Apparatus
14.1 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
(H SO ).
20.1 Viscometer, Rotational type.
2 4
NOTE 1—Manufacturers of cellulose derivatives usually specify the
15. Procedure
viscometer make, model, spindle, and speed to be used with their
15.1 Weigh, to the nearest 0.0001 g, about2gofthe dried
products. It is highly recommended that these specifications be followed.
sample into a tared platinum dish. Moisten the entire specimen
Use of a viscometer made by another company or even a different model
with about 2 mL of H SO . Then cautiously heat over a small
by the same company will result in slightly different results.
2 4
flame until sulfur trioxide (SO ) fumes cease to be evolved. 3
20.2 Container, glass jar, 350-cm approximately 64 mm in
15.2 Increase the heat, ignite the specimen, and heat as
outside diameter and 152 mm high.
necessary to burn off the volatile matter. Avoid spattering.
20.3 Mechanical Stirrer—Agitator as shown in Fig. 1 or
15.3 Place the dish in a 825°C muffle furnace for 1 h, or 6
Fig. 2, attached to a variable-speed motor capable of 1500
longer if required, to burn all of the carbon.
r/min.
15.4 Remove the dish, allow to cool somewhat, place in a
20.4 Water Bath, constant-temperature, set at 25°C and
desiccator, and cool to room temperature. Weigh the dish and
capable of maintaining that temperature to within 60.2°C.
residue to the nearest 0.0001 g.
20.5 Thermometer—An ASTM Saybolt Viscosity Ther-
mometer having a range from 19 to 27°C and conforming to
16. Calculation
the requirements for Thermometer 17C, as prescribed in
16.1 Calculate the percent of ash (as sulfate), C, as follows:
Specification E 1.
C 5 ~A/B!3 100 (2)
An agitator made with 1 1/2 in. (38 mm), three-bladed propellers, No. 9240K,
available from A. H. Thomas Co., P.O. Box 779, Philadelphia, PA 19105 has been
where:
found satisfactory for this purpose.
A = ash, g, and
B = sample used, g.
TABLE 1 Viscometer Spindles Required for Given Speeds
Viscosity Range,
17. Precision and Bias Spindle No. Speed, rpm Scale Factor
cP
17.1 Statistical analysis of interlaboratory (reproducibility)
10 to 100 1 60 100 1
test results on samples containing 2 to 5 % ash (as sulfate) 100 to 200 1 30 100 2
200 to 1000 2 30 100 10
indicates a precision of 60.3 % absolute at the 95 % level.
1000 to 4000 3 30 100 40
17.2 No statement on bias can be made as no suitable
4000 to 10 000 4 30 100 200
reference material is available as a standard.
D 2364
in. mm in. mm
1 5
⁄16 1.5 ⁄16 7.9
3 5
⁄16 4.8 ⁄8 15.8
1 1
⁄4 6.4 1 ⁄2 38
9 1
⁄32 79 ⁄2 241
FIG. 1 Agitator
21. Procedure
21.1 Determine the moisture in accordance with Sections
4-9.
21.2 Calculate the dry-basis specimen mass, M, in grams
necessary to make 250 g of test solution as follows:
M 5 100 A/~100 – B! (3)
s
where:
A = desired dry mass of specimen, g, and
B = percent moisture in the weighed specimen.
21.3 Add the specimen to the jar. Then add sufficient
distilled water to make a total of 250 g of solution. Calculate
the mass of water, M , in grams as follows:
W
M 5 250 – S (4)
w
where S = sample mass, g.
21.4 Place the agitator in the solution allowing a minimum
clearance between the agitator and the bottom of the container.
Stir at approximately 1500 r/min until the specimen is com-
pletely dissolved. This may require several hours.
21.5 Remove the agitator from the motor and transfer the
specimen container, with the agitator in it, to the constant
temperature bath. Allow it to stand for 1 h.
21.6 Remove the specimen container from the bath and
shake or stir vigorously for 10 s. Measure the viscosity with the
rotational viscometer, following the manufacturer’s instruc-
tions, selecting the proper spindle and speed from Table 1.
Allow the spindle to rotate for 3 min before taking a reading.
NOTE 2—If the room temperature is considerably greater or less than
FIG. 2 Agitator
25°C, the entire operation of stirring, standing, and measurement should
be conducted with the specimen suspended in the water bath.
D 2364
NOTE 3—Shaking or stirring the sample may cause entrainment of air
breakage, cover the tapping surface witha3to 6-mm thick
bubbles. Caution: One must exercise care to avoid having a large air
rubber sheet, or use a plastic graduated cylinder.
bubble under the viscometer spindle when taking the measurement.
30. Calculation
22. Calculation
30.1 Calculate the density, D, in grams per millilitre as
22.1 Calculate the viscosity, V, in centipoises as follows:
follows:
V 5 r 3 f (5)
D 5 50/r (6)
o
where:
where R = observed reading, mL.
o
r = reading and
31. Precision and Bias
f = factor.
31.1 Precision—Statistical analysis of intralaboratory (re-
23. Report
peatability) test results indicates a precision of 60.04 g/mL at
23.1 Report the following information:
the 95 % confidence level.
23.1.1 Results, as viscosity at 25°C,
31.2 Bias—No justifiable statement on the bias of the
23.1.2 Solution concentration,
procedure for measuring density can be made because no
23.1.3 Spindle used, and
suitable reference material exists.
23.1.4 Speed used.
MOLAR SUBSTITUTION
24. Precision and Bias
32. Scope
24.1 Precision—Statistical analysis of interlaboratory (re-
producibility) test results indicates a precision of 610 % at the 32.1 This test method covers the determination of the molar
95 % confidence level when using the same viscometer make substitution (MS) of hydroxyethyloxyethylene pendant groups
and model. in purified hydroxyethylcellulose (HEC).
32.2 An alternative preferred method is found in Test
24.2 Bias—No justifiable statement can be made on the bias
of the procedure for measuring viscosity because no suitable Method D 4794.
reference material exists.
33. Terminology
DENSITY
33.1 Definitions:
33.1.1 molar substitution, MS—the average number of oxy-
25. Scope
ethylene groups substituted onto each anhydroglucose unit (see
25.1 This test method covers the determination of the bulk
also Terminology D 1695).
density of hydroxyethylcellulose.
34. Summary of Test Method
26. Summary of Test Method
34.1 In this test method, the pendant groups are cleaved
26.1 A weighed amount of hydroxyethylcellulose is trans-
from the cellulose by hydriodic acid and converted to volatile
ferred to a 100-mL graduated cylinder and the graduate
ethyl iodide and ethylene. These volatile products are collected
vibrated to settle the powder.
in alcoholic silver nitrate and bromine-bromide scrubbers,
respectively. The total hydroxyethyl content is calculated on
27. Significance and Use
the basis of the sum of both products.
27.1 Density can relate to dry flow properties, rate of
dissolution, lumping, packaging, and storage space require-
35. Significance and Use
ments.
35.1 This test method determines the amount of substituent
groups added to the cellulose backbone. The level can affect
28. Apparatus
solution properties, rheology, solubility parameters, and film
28.1 Vibrator—A magnetic-type electric vibrator attached
properties.
to the vertical support rod of a ring stand approximately 0.3 m
above the base. A condenser clamp of sufficient size to hold a
36. Interferences
100-mL graduated cylinder also shall be attached to the above
36.1 Interfering materials include glycols, low molecular
rod. The base of the stand should be weighted.
weight alcohols, and salts of oxidizing acids. Presence of
glycols or alcohols, or both, leads to high MS values since
29. Procedure
reaction of these compounds with hydriodic acid is similar to
29.1 Place 50.0 g of hydroxyethylcellulose in a 100-mL
that of HEC. If present, they must be either removed or
graduated cylinder and place in the condenser clamp. Turn on
determined separately with the results being included in the
the vibrator and allow the cylinder to vibrate for 3 min. Record
MS calculations. Large amounts of salts of oxidizing acids also
the level (in millilitres) to which the specimen has compacted.
interfere giving low MS values. If any such salt is present in
29.2 Alternatively, the specimen may be compacted manu-
ally. Tap it on a hard surface by dropping the cylinder
repeatedly from a height of about 25 mm until the volume of
This test method was first published by Morgan, P. W. in Industrial and
the sample remain
...
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