ASTM D5400-03(2013)

Standard Test Methods for Hydroxypropylcellulose

SIGNIFICANCE AND USE
5.1 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.  
5.2 Moisture analysis (along with residue on ignition) is a measure of the amount of active polymer in the material and must be considered when determining the amount of hydroxypropylcellulose to use in various formulations.
SCOPE
1.1 These test methods cover the testing of hydroxypropylcellulose.  
1.2 The test procedures appear in the following order:
Sections  
Moisture  
4-9  
Viscosity  
10-16  
pH  
17-21  
Residue on Ignition  
22-28  
Hydroxypropoxy Content  
29-36
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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 appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see 26.6.

General Information

• Status: Historical
• Publication Date: 31-May-2013
• ICS: 85.040 - Pulps
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Replaces: ASTM D5400-03(2008) - Standard Test Methods for Hydroxypropylcellulose
• Effective Date: 01-Jun-2013

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D5400 −03(Reapproved 2013)
Standard Test Methods for
Hydroxypropylcellulose
This standard is issued under the fixed designation D5400; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
1.1 These test methods cover the testing of hydroxypropy-
sufficiently high purity to permit its use without lessening the
lcellulose.
accuracy of the determination.
1.2 The test procedures appear in the following order:
3.2 Purity of Water—Unless otherwise indicated, references
Sections
to water shall be understood to mean distilled water.
Moisture 4–9
Viscosity 10–16
MOISTURE
pH 17–21
Residue on Ignition 22–28
Hydroxypropoxy Content 29–36
4. Scope
1.3 The values stated in SI units are to be regarded as the
4.1 Thistestmethodcoversthedeterminationofthevolatile
standard. The values given in parentheses are for information
content of hydroxypropylcellulose.
only.
5. Significance and Use
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.1 The results of this test are used for calculating the total
responsibility of the user of this standard to establish appro-
solids in the sample; and, by common usage, all materials
priate safety and health practices and determine the applica- volatile at this test temperature are designated as moisture.
bility of regulatory limitations prior to use. For specific hazard
5.2 Moisture analysis (along with residue on ignition) is a
statements, see 26.6.
measure of the amount of active polymer in the material and
must be considered when determining the amount of hydroxy-
2. Referenced Documents
propylcellulose to use in various formulations.
2.1 ASTM Standards:
6. Apparatus
D3876Test Method for Methoxyl and Hydroxypropyl Sub-
stitution in Cellulose Ether Products by Gas Chromatog- 6.1 Oven, gravity convection, capable of maintaining a
raphy
temperature of 105 6 3°C.
E70Test Method for pH of Aqueous Solutions With the
6.2 Weighing Dish, glass or aluminum, with cover, 50 mm
Glass Electrode
in diameter, 25 mm in height, or equivalent.
6.3 Analytical Balance.
3. Reagents
3.1 Purity of Reagents—Reagent grade chemicals shall be
7. Procedure
used in all tests. Unless otherwise indicated, it is intended that
7.1 Weigh about5gof sample to the nearest 0.001 g in a
all reagents shall conform to the specifications of the Commit-
tared and covered weighing dish.
tee onAnalytical Reagents of theAmerican Chemical Society,
7.2 Place it in an oven at 105 6 1°C for 3 h with the cover
removed.
7.3 Removethedishfromtheoven,immediatelyreplacethe
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct cover, cool in a desiccator, and weigh.
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved June 1, 2013. Published June 2013. Originally
approved in 1993. Last previous edition approved in 2008 as D5400–03(2008). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D5400-03R13. 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 [e-mail]. 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
D5400−03 (2013)
A
TABLE 1 Brookfield Viscometer Spindle and Speed
11.2 This test method determines the relative ability of the
Combinations
polymertothickenaqueoussolutionsandisthereforerelatedto
Viscosity Range, Spindle Speed,
Scale Factor the concentration required in various formulations to achieve
cP Number r/min
the desired finished product viscosity.
10–80 1 60 100 1
20–160 1 30 100 2
50–400 2 60 100 5
12. Apparatus
100–800 2 30 100 10
12.1 Viscometer, Brookfield Type.
400–1600 3 60 100 20
800–3200 3 30 100 40
12.2 Container,glassbottle,350-cm (12-oz)approximately
2000–8000 4 60 100 100
4000–16 000 4 30 100 200 64 mm (2 ⁄2 in.) in outside diameter and 152 mm (6 in.) high.
A 4
Brookfield Viscometer, Model LVF .
12.3 Mechanical Stirrer, agitator as shown in Fig. 1, at-
tached to a variable-speed motor capable of 1500 r/min.
12.4 Water Bath, constant-temperature, set at 25°C and
8. Calculation capable of maintaining that temperature to within 60.5°C.
8.1 Calculate the percent moisture, M, as follows:
13. Procedure
M 5 ~A/B! 3100 (1)
13.1 Determine the moisture in accordance with Sections 4
where: –9.
A = mass loss on heating, g, and
13.2 Calculate the sample mass, S, in grams necessary to
B = sample used, g.
make 250 g of test solution as follows:
8.2 Report the moisture content to the nearest 0.1%.
A 3100
S 5 (2)
100 2 B
9. Precision and Bias
where:
9.1 Precision—Statistical analysis of intralaboratory test
A = desired dry mass of sample, g, and
resultsonsamplescontainingfrom1to6%moistureindicates
B = percent moisture in the weighed sample.
a precision of 60.2% absolute at the 95% confidence level.
13.3 Calculate the mass of water required, W, in grams as
9.2 Bias—No justifiable statement on bias can be made as
follows:
no suitable reference material is available as a standard.
VISCOSITY
10. Scope
10.1 This test method is an arbitrary method of determining
theviscosityofaqueoussolutionsofhydroxypropylcellulosein
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
agreed upon between the purchaser and the seller. It shall be
such that the viscosity of the solution will fall within the range
of this test.
10.3 The results for the viscosity of hydroxypropylcellulose
bythistestmethodwillnotnecessarilycheckwithresultsfrom
other types of instruments used for viscosity measurement.
10.4 The determinations are run on a calculated dry basis;
that is, the amount of hydroxypropylcellulose required for the
desired concentration on a dry basis is calculated from the
known moisture content.
11. Significance and Use
11.1 This test method is intended for referee purposes. The
Brookfield spindles and speeds given in Table 1 are recom-
mended for this purpose, but slight deviations from Table 1
may occasionally be found convenient for individual applica-
tion.
Model LVF, available from Brookfield Engineering Laboratories, Inc.,
Stoughton, MA has been found satisfactory for this purpose. FIG. 1 Stainless Steel Agitator
D5400−03 (2013)
W 5 250 2 S (3) must be taken into consideration when determining materials
of construction for equipment and packaging for handling and
where:
storing these solutions. Also, pH may affect suitability for
S = sample mass, g.
certain end-use applications.
13.4 Weighthewaterintotheglassbottleandplaceitonthe
19. Apparatus
stirrer,mixingataspeedsufficienttocauseavortexbutnotfast
enough to splash.
19.1 pH Meter, with glass electrodes.
13.5 Sprinkle the hydroxypropylcellulose sample into the
20. Procedure
water slowly, to prevent lumping. Increase stirring speed to
approximately 900 6 100 r/min and stir until the sample is
20.1 Determine the pH of the viscosity solution from 13.5,
completely dissolved (1 to 2 h).
usingasuitablepHmeterthathasbeenstandardizedaccording
to Test Method E70.
13.6 Removetheglassbottlefromthestirrer,capthebottle,
and place it in the constant temperature bath for 30 min or as
21. Precision and Bias
long as necessary to bring the solution to 25 6 0.5°C.
21.1 Precision—Statistical analysis of intralaboratory test
13.7 Removetheglassbottlefromthewaterbathandinvert
results on samples with pH values of 4.5 to 8.5 indicates a
it slowly 4 to 5 times, taking care to minimize the introduction
precision of 65% at the 95% confidence level.
of air bubbles.
21.2 Bias—No justifiable statement on bias can be made as
13.8 Measure the viscosity with the Brookfield viscometer,
no suitable reference material is available as a standard.
following the manufacturer’s operating instructions. Select the
proper spindle and speed from Table 1. Allow the spindle to
RESIDUE ON IGNITION
rotate for 3 min before taking the reading. Use the spindle
guard.
22. Scope
NOTE 1—If the room temperature is considerably greater or less than
22.1 This test method covers the determination of the
25°C; the entire operation of stirring, standing, and measurement should
amount of residue left from igniting a sample of hydroxypro-
be conducted with the glass bottle suspended in the constant temperature
pylcellulose after being moistened first with sulfuric acid and
bath.
then with hydrofluoric acid.
14. Calculation
14.1 Calculate the viscosity, V, in centipoises as follows: 23. Significance and Use
V 5 r 3 f (4)
23.1 Excessiveresidueonignitioncanaffectsolutionclarity
and film properties. The residue on ignition (along with
where:
moisture) is a measure of the amount of active polymer in the
r = scale reading and
materialandmustbeconsideredwhendeterminingtheamount
f = factor from Table 1.
of hydroxypropylcellulose to use in various formulations.
15. Report
23.2 Commercially available hydroxypropylcellulose most
often has up to 0.60% silica added as an anti-caking agent.
15.1 Report the following information:
Therefore, a hydrofluoric acid ashing step is required to
15.1.1 Results, as Brookfield viscosity at 25°C,
remove the silica.
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