ASTM D5400-93(1997)
(Test Method)Standard Test Methods for Hydroxypropylcellulose
Standard Test Methods for Hydroxypropylcellulose
SCOPE
1.1 These test methods cover the testing of hydroxypropylcellulose.
1.2 The test procedures appear in the following order: Sections Moisture 4 to 9 Viscosity 10 to 16 pH 17 to 21 Residue on Ignition 22 to 28 Hydroxypropoxy Content 29 to 36
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. For specific hazard statements, see Note 2.
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Designation: D 5400 – 93 (Reapproved 1997)
Standard Test Methods for
Hydroxypropylcellulose
This standard is issued under the fixed designation D 5400; 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 sufficiently high purity to permit its use without lessening the
accuracy of the determination.
1.1 These test methods cover the testing of hydroxypropy-
3.2 Purity of Water—Unless otherwise indicated, references
lcellulose.
to water shall be understood to mean distilled water.
1.2 The test procedures appear in the following order:
Sections
MOISTURE
Moisture 4 to 9
Viscosity 10 to 16
4. Scope
pH 17 to 21
Residue on Ignition 22 to 28
4.1 This test method covers the determination of the volatile
Hydroxypropoxy Content 29 to 36
content of hydroxypropylcellulose.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.1 The results of this test are used for calculating the total
priate safety and health practices and determine the applica-
solids in the sample; and, by common usage, all materials
bility of regulatory limitations prior to use. For specific hazard
volatile at this test temperature are designated as moisture.
statements, see Note 2.
5.2 Moisture analysis (along with residue on ignition) is a
measure of the amount of active polymer in the material and
2. Referenced Documents
must be considered when determining the amount of hydrox-
2.1 ASTM Standards:
ypropylcellulose to use in various formulations.
D 3876 Test Method for Methoxyl and Hydroxypropyl
6. Apparatus
Substitution in Cellulose Ether Products by Gas Chroma-
tography
6.1 Oven, gravity convection, capable of maintaining a
E 70 Test Method for pH of Aqueous Solutions With the
temperature of 105 6 3°C.
Glass Electrode
6.2 Weighing Dish, glass or aluminum, with cover, 50 mm
in diameter, 25 mm in height, or equivalent.
3. Reagents
6.3 Analytical Balance.
3.1 Purity of Reagents—Reagent grade chemicals shall be
7. Procedure
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
7.1 Weigh about5gof sample to the nearest 0.001 g in a
tee on Analytical Reagents of the American Chemical Society,
tared and covered weighing dish.
where such specifications are available. Other grades may be
7.2 Place it in an oven at 105 6 1°C for 3 h with the cover
used, provided it is first ascertained that the reagent is of
removed.
7.3 Remove the dish from the oven, immediately replace the
cover, cool in a desiccator, and weigh.
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
8. Calculation
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved May 15, 1993. Published July 1993.
8.1 Calculate the percent moisture, M, as follows:
Annual Book of ASTM Standards, Vol 06.03.
M 5 ~A/B! 3 100 (1)
Annual Book of ASTM Standards, Vol 15.05.
Reagent Chemicals, American Chemical Society Specifications, American
where:
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
A = mass loss on heating, g, and
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5400 – 93 (1997)
12.2 Container, glass bottle, 12-oz (350-cm ) approxi-
B = sample used, g.
mately 2 ⁄2 in. (64 mm) in outside diameter and 6 in. (152 mm)
8.2 Report the moisture content to the nearest 0.1 %.
high.
9. Precision and Bias 12.3 Mechanical Stirrer, agitator as shown in Fig. 1, at-
tached to a variable-speed motor capable of 1500 r/min.
9.1 Precision—Statistical analysis of intralaboratory test
12.4 Water Bath, constant-temperature, set at 25°C and
results on samples containing from 1 to 6 % moisture indicates
capable of maintaining that temperature to within 6 0.5°C.
a precision of 60.2 % absolute at the 95 % confidence level.
9.2 Bias—No justifiable statement on bias can be made as
13. Procedure
no suitable reference material is available as a standard.
13.1 Determine the moisture in accordance with Sections
VISCOSITY
4-9.
13.2 Calculate the sample mass, S, in grams necessary to
10. Scope
make 250 g of test solution as follows:
10.1 This test method is an arbitrary method of determining
A 3 100
S 5 (2)
the viscosity of aqueous solutions of hydroxypropylcellulose in
100 2 B
the viscosity range of 10 to 16 000 cP/s at 25°C.
10.2 The concentration to be used for the test shall be
where:
agreed upon between the purchaser and the seller. It shall be
A = desired dry mass of sample, g, and
such that the viscosity of the solution will fall within the range
B = percent moisture in the weighed sample.
of this test.
13.3 Calculate the mass of water required, W, in grams as
10.3 The results for the viscosity of hydroxypropylcellulose
follows:
by this test method will not necessarily check with results from
W 5 250 2 S (3)
other types of instruments used for viscosity measurement.
10.4 The determinations are run on a calculated dry basis;
where:
that is, the amount of hydroxypropylcellulose required for the
S = sample mass, g.
desired concentration on a dry basis is calculated from the
13.4 Weigh the water into the glass bottle and place it on the
known moisture content.
stirrer, mixing at a speed sufficient to cause a vortex but not fast
enough to splash.
11. Significance and Use
13.5 Sprinkle the hydroxypropylcellulose sample into the
11.1 This test method is intended for referee purposes. The
water slowly, to prevent lumping. Increase stirring speed to
Brookfield spindles and speeds given in Table 1 are recom-
A
TABLE 1 Brookfield Viscometer Spindle and Speed
Combinations
Viscosity Range, Spindle Speed,
Scale Factor
cP Number r/min
10–80 1 60 100 1
20–160 1 30 100 2
50–400 2 60 100 5
100–800 2 30 100 10
400–1600 3 60 100 20
800–3200 3 30 100 40
2000–8000 4 60 100 100
4000–16 000 4 30 100 200
A 5
Brookfield Viscometer, Model LVF .
mended for this purpose, but slight deviations from Table 1
may occasionally be found convenient for individual applica-
tion.
11.2 This test method determines the relative ability of the
polymer to thicken aqueous solutions and is therefore related to
the concentration required in various formulations to achieve
the desired finished product viscosity.
12. Apparatus
12.1 Viscometer, Brookfield Type.
Model LVF, available from Brookfield Engineering Laboratories, Inc., Stough-
ton, MA has been found satisfactory for this purpose. FIG. 1 Stainless Steel Agitator
D 5400 – 93 (1997)
approximately 900 6 100 r/min and stir until the sample is 21. Precision and Bias
completely dissolved (1 to 2 h).
21.1 Precision—Statistical analysis of intralaboratory test
13.6 Remove the glass bottle from the stirrer, cap the bottle,
results on samples with pH values of 4.5 to 8.5 indicates a
and place it in the constant temperature bath for 30 min or as
precision of 65 % at the 95 % confidence level.
long as necessary to bring the solution to 25 6 0.5°C.
21.2 Bias—No justifiable statement on bias can be made as
13.7 Remove the glass bottle from the water bath and invert
no suitable reference material is available as a standard.
it slowly 4 to 5 times, taking care to minimize the introduction
of air bubbles.
RESIDUE ON IGNITION
13.8 Measure the viscosity with the Brookfield viscometer,
22. Scope
following the manufacturer’s operating instructions. Select the
proper spindle and speed from Table 1. Allow the spindle to
22.1 This test method covers the determination of the
rotate for 3 min before taking the reading. Use the spindle
amount of residue left from igniting a sample of hydroxypro-
guard.
pylcellulose after being moistened first with sulfuric acid and
then with hydrofluoric acid.
NOTE 1—If the room temperature is considerably greater or less than
25°C; the entire operation of stirring, standing, and measurement should
23. Significance and Use
be conducted with the glass bottle suspended in the constant temperature
bath.
23.1 Excessive residue on ignition can affect solution clarity
and film properties. The residue on ignition (along with
14. Calculation
moisture) is a measure of the amount of active polymer in the
14.1 Calculate the viscosity, V, in centipoises as follows:
material and must be considered when determining the amount
V 5 r 3 f (4)
of hydroxypropylcellulose to use in various formulations.
23.2 Commercially available hydroxypropylcellulose most
where:
often has up to 0.60 % silica added as an anti-caking agent.
r = scale reading and
Therefore, a hydrofluoric acid ashing step is required to
f = factor from Table 1.
remove the silica.
15. Report
24. Apparatus
15.1 Report the following information:
24.1 Dishes, platinum, 75-mL capacity.
15.1.1 Results, as Brookfield viscosity at 25°C,
15.1.2 Solution concentration, 24.2 Hot Plate.
24.3 Muffle Furnace, capable of reaching 1000 6 25°C.
15.1.3 Spindle used, and
15.1.4 Speed used.
25. Reagents
16. Precision and Bias
25.1 Sulfuric Acid, (sp gr 1.84)—concentrated sulfuric acid
16.1 Precision—Statistical analysis of interlaboratory test
(H SO ).
2 4
results indicates a precision of 610 % at the 95 % confidence
25.2 Hydrofluoric Acid (48 %).
level.
16.2 Bias—No j
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