ASTM D2363-79(1995)e1

Standard Test Methods for Hydroxypropyl Methylcellulose

SCOPE
1.1 These test methods cover the testing of hydroxypropyl methylcellulose.
1.2 The test procedures appear in the following order: SectionsMoisture4 to 6Ash (as Sulfate)7 to 10Chlorides (as NaCl)11 to 14Alkalinity (as Na2CO3)15 to 18Iron 19 to 24Heavy Metals25 to 29Methoxyl Content30 to 35Hydroxypropoxyl Content36 to 41Viscosity42 to 46pH 47Solids 48 to 51Density 52 to 56
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 a specific hazard statement, see 33.5.1.

General Information

• Status: Historical
• Publication Date: 31-Dec-1999
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Replaced By: ASTM D2363-79(2000)e1 - Standard Test Methods for Hydroxypropyl Methylcellulose
• Effective Date: 01-Jan-2000

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 2363 – 79 (Reapproved 1995)
Standard Test Methods for
Hydroxypropyl Methylcellulose
This standard is issued under the fixed designation D 2363; 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.
e NOTE—Editorial changes were made throughout in October 1995.
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 hydroxypropyl
vided it is first ascertained that the reagent is of sufficiently
methylcellulose.
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, references to water shall be
Moisture 4 to 6
understood to mean distilled water.
Ash (as Sulfate) 7 to 10
Chlorides (as NaCl) 11 to 14
MOISTURE
Alkalinity (as Na CO ) 15to18
2 3
Iron 19 to 24
4. Scope
Heavy Metals 25 to 29
Methoxyl Content 30 to 35
4.1 This test method covers the determination of the volatile
Hydroxypropoxyl Content 36 to 41
content of hydroxypropyl methylcellulose and, by common
Viscosity 42 to 46
pH 47
usage, designated moisture.
Solids 48 to 51
Density 52 to 56
5. Procedure
1.3 The values stated in inch-pound units are to be regarded
5.1 Transfer 2 to5gofthe sample weighed to the nearest
as the standard. The values given in parentheses are for
0.01 g to a tared dish (fitted with a lid) and dry for2hinan
information only.
oven at 100 to 105°C with lid removed. Remove the dish from
1.4 This standard does not purport to address all of the
the oven, cover with a lid, cool in a desiccator, and weigh.
safety concerns, if any, associated with its use. It is the
6. Calculation
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6.1 Calculate the percent of moisture as follows:
bility of regulatory limitations prior to use. For a specific
Moisture, % 5 A/B! 3 100 (1)
~
hazard statement, see Note 1.
where:
2. Referenced Documents
A 5 mass loss on heating, and
2.1 ASTM Standards: B 5 sample used, g.
D 96 Test Methods for Water and Sediment in Crude Oil by
ASH—AS SULFATE
Centrifuge Method (Field Procedure)
E 70 Test Method for pH of Aqueous Solutions With the
7. Scope
Glass Electrode
7.1 This test method covers the determination of the amount
of residue left from igniting a sample of hydroxypropyl
3. Purity of Reagents
methylcellulose after being moistened with sulfuric acid.
3.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
8. Reagents
conform to the specifications of the Committee on Analytical
8.1 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
(HNO ).
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and are the direct responsibility
Reagent Chemicals, American Chemical Society Specifications, American
of Subcommittee D01.36 on Cellulosics. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved May 25, 1979. Published July 1979. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 2363 – 65 T. Last previous edition D 2363 – 72. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 05.01. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.05. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 2363
8.2 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
B 5 KCNS solution required for the titration, mL.
(H SO ).
2 4 12.4 Silver Nitrate-Standard Solution (0.100 N)—Grind
silver nitrate (AgNO ) crystals fine enough to pass through a
9. Procedure
No. 20 (850-μm) sieve and then dry for2hat110°C. Prepare
9.1 Weigh to the nearest 0.01 g about2gofthe sample
a 0.100 N solution by dissolving 16.989 g of dry AgNO in
(previously dried for ⁄2 h at 105°C) into a tared Coors No. 1,
chloride-free water and diluting to 1 L in a volumetric flask.
high-form, porcelain crucible. Add 5 drops of H SO around
2 4
13. Procedure
the inside surface of the crucible. Place the crucible inside of a
loosely fitting aluminum ring (approximately 1 ⁄4 in. (32 mm) 13.1 Weigh to the nearest 0.01 g about 1.0 g of the sample
1 3 1
(previously dried for ⁄2 h at 100 to 105°C) and transfer to a
high, with ⁄4-in. (6.4-mm) sidewall, and 1 ⁄4-in. (44-mm)
inside diameter, cut from a piece of aluminum pipe) on a hot 500-mL, wide-mouth Erlenmeyer flask. Add 250 mL of hot
water and swirl for a few minutes; then cool to dissolve.
plate. Loosely cover with a crucible cover. Carefully char the
hydroxypropyl methylcellulose until all the volatiles are re- 13.2 Add 5 mL of 0.100 N AgNO solution and 5 mL of
ferric alum indicator solution, and back-titrate with 0.1 N
moved.
9.2 Cool the crucible, add 1 ml of H SO and2mlofHNO KCNS solution to the first appearance of a faint pink color.
2 4 3
so that it completely wets the charred residue. Cautiously heat
14. Calculation
to dense white fumes on a hot plate. Place the uncovered
14.1 Calculate the percent of chlorides as NaCl as follows:
crucible in a muffle furnace at 600°C and ignite until all the
carbon is gone (for about 1 h). Transfer to a dessicator until Chlorides, % 5 ~@~AB 2 CD! 3 0.0585#/E! 3 100 (4)
cool, then weigh. (Save the residue for the Heavy Metals
where:
determination.)
A 5 AgNO solution added, mL,
B 5 normality of the AgNO solution,
10. Calculation 3
C 5 KCNS solution required to back-titrate the excess
10.1 Calculate the percent of ash, C, as follows:
AgNO , mL,
C 5 ~A/B! 3 100 (2)
D 5 normality of the KCNS solution, and
E 5 sample used, g.
where:
ALKALINITY—AS SODIUM CARBONATE
A 5 sulfated ash, g, and
B 5 sample used, g.
15. Scope
CHLORIDES—AS SODIUM CHLORIDE 15.1 This test method covers the determination of the total
alkalinity of hydroxypropyl methylcellulose expressed as so-
11. Scope
dium carbonate (Na CO ).
2 3
11.1 This test method covers the determination of the total
16. Reagents
percent of chloride (bromide included if present) calculated as
16.1 Methyl Purple Indicator Solution.
sodium chloride (NaCl) in hydroxypropyl methylcellulose. The
16.2 Sulfuric Acid, Standard (0.01 N)—Prepare and stan-
sample is dispersed and the chloride titrated volumetrically
dardize a 0.01 N solution of sulfuric acid (H SO ).
with 0.100 N silver nitrate solution. 2 4
17. Procedure
12. Reagents
17.1 Weigh to the nearest 0.01 g about 1.0 g of the sample
12.1 Ferric Alum Indicator Solution—Add 100 g of ferric
(previously dried for ⁄2 h at 100 to 105°C) and transfer to a
ammonium sulfate FeNH (SO ) ·12H O to 250 mL of water.
4 4 2 2
500-ml, widemouth Erlenmeyer flask. Add 250 mL of hot
Heat to boiling and add NHO (sp gr 1.42) slowly until the red
water and swirl for a few minutes; then cool to dissolve.
color is removed. This will usually require about 6 to 15 mL of
17.2 Add 4 drops of methyl purple indicator solution and
HNO . Filter the solution and store in a glass bottle.
titrate to the first faint pink color with 0.01 N H SO .
2 4
12.2 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
(HNO ). 18. Calculation
12.3 Potassium Thiocyanate Standard Solution (0.1 N)—
18.1 Calculate the percent alkalinity as Na CO , S,as
2 3
Dissolve 10 g of potassium thiocyanate (KCNS) in 1 L of
follows:
water. By means of a pipet, measure 25 mL of 0.100 N silver
S 5 @~AB 3 0.053!/C# 3 100 (5)
nitrate (AgNO ) solution into a 400-mL beaker. Add 100 mL of
water, 10 mL of HNO (sp gr 1.42), and 5 mL of ferric alum
3 where:
indicator solution. Titrate with the KCNS solution, while
A 5 H SO required for titration of the sample, mL,
2 4
stirring, until a faint persistent red color is produced. Calculate
B 5 normality of the H SO , and
2 4
the normality, N, of the KCNS solution as follows: C 5 sample used, g.
N 5 A/B 3 0.1 (3)
~ !
IRON
where:
19. Scope
A 5 0.100 N AgNO solution added, mL, and
19.1 This test method covers the determination of total iron
D 2363
content in samples of hydroxypropyl methylcellulose. The iron 23.3 Add 2 mL of the color-forming solution described in
is converted to ferric sulfate which reacts with the indicator to 21.3, and mix. Adjust pH to 7.0 and then dilute to mark with
form a pink color that can be quantitatively measured. buffer. Transfer a small portion to an absorption cell and
determine the photometer reading at 480 nm.
20. Apparatus
23.4 Blank—Make a blank determination, using the same
20.1 Photometer—Any photoelectric filter photometer or amount of reagents and the same procedure as for the sample.
spectrophotometer suitable for measurements at 430 nm.
24. Calculation
20.2 Kjeldahl Flasks—Calibrated to contain 50 mL, and
24.1 Read the iron content, in parts per million, directly
made of heat- and chemical-resistant glass.
from the calibration curve (Section 22). Subtract the parts per
21. Reagents
million of iron due to iron in the blank.
21.1 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
HEAVY METALS
monium hydroxide (NH OH).
21.2 Buffer Solution—Dissolve 20 g of sodium bicarbonate
25. Scope
(NaHCO ) and 10 g of sodium carbonate (Na CO ) in water
3 2 3
25.1 This test method covers the determination of whether
and dilute to 1 L.
or not the heavy metals content of hydroxypropyl methylcel-
21.3 Disodium-1,2-Dihydroxybenzene-3,5-Disulfonate
lulose is below a given level based on a lead standard.
Solution —Prepare an aqueous solution containing 25 g/L.
26. Summary of Test Method
21.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
chloric acid (HCl).
26.1 The ash residue from the sulfated ash test is digested
21.5 Hydrogen Peroxide (30 %)—Concentrated hydrogen
with dilute hydrochloric acid. A standard containing a known
peroxide (H O ).
2 2 amount of lead is prepared, and the heavy metals content is
21.6 Iron Standard Solution (0.0001 g Fe/ml)—Dissolve
determined qualitatively by comparing the sample to the
0.01 g of iron powder containing not less than 99.9 % iron in
standard.
HCl (sp gr 1.19). Oxidize the solution with bromine water and
27. Apparatus
expel the excess by boiling. Dilute to 1 L in a volumetric flask.
21.7 Phenolphthalein Indicator Solution (1 g/100 mL)— 27.1 Nessler Tubes, 50-mL.
Dissolve1gof phenolphthalein in 100 mL of ethanol (95 %).
27.2 Volumetric Flasks, 50-mL.
21.8 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
28. Reagents
(H SO ).
2 4
21.9 Sulfuric Acid (1+4)—Carefully mix 1 volume of 28.1 Acetic Acid—Glacial acetic acid.
28.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
H SO (sp gr 1.84) with 4 volumes of water, adding the H SO
4 2 4
monium hydroxide (NH OH).
gradually while mixing.
28.3 Ammonium Hydroxide (2+3)—Dilute 400 mL of
22. Preparation of Calibration Curve
NH OH (sp gr 0.90) with sufficient water to make 1000 mL.
28.4 Buffer Solution—Dissolve 60 mL of acetic acid in
22.1 Following the procedure given in Section 23, and using
about 500 mL of water, add 10 mL of NH OH, and dilute to 1
varied amounts of the standard iron solution prepared in
L.
accordance with 21.6, prepare a calibration curve showing iron
28.5 Hydrochloric Acid (1+2)—Dilute 1 volume of concen-
content in parts per million and the corresponding photometer
trated hydrochloric acid (HCl, sp gr 1.19) with 2 volumes of
readings.
water.
23. Procedure
28.6 Hydrogen Sulfide TS—Saturate a convenient volume of
water with hydrogen sulfide (H S) in a narrow-neck, glass-
23.1 Weigh to the nearest 0.01 g about2gofthe sample 2
stoppered, amber bottle. This solution must be made fresh.
(previously dried for ⁄2 h at 100 to 105°C). Transfer by means
28.7 Hydroxylamine Hydrochloride Solution (200 g/L)—
of a funnel to a Kjeldahl flask. Place the flask at a 20° angle in
Dissolve 20 g of hydroxylamine hydrochloride (NH OH·HCl)
the furnace at 500°C and heat until some charring of the sample
in 100 mL of water.
has taken place. (Care must be taken not to char too much.)
28.8 Lead Nitrate Stock Solution—Dissolve 159.8 mg of
Remove and allow to cool.
lead nitrate (Pb(NO ) ) in 100 mL of water containing 1 mL of
23.2 Add 3 mL of H SO to the flask. Place on the digestion 3 2
2 4
HNO (sp gr 1.42). Dilute with water to 1000.0 mL and mix.
rack and digest. Cool and add H O dropwise until the solution
2 2
This solution should be prepared and stored in glass containers
is clear. Heat over a Meker burner to a volume of 2 mL. Cool,
that are free from lead salts.
and wash the sides of the flask with water. Add 3 drops of
28.9 Lead Standard Solution (1mL 51μgPb)—Dilute 10
phenolphthalein indicator solution. Add NH OH to a red end
mL of the lead nitrate stock solution, accurately measured, with
point. Wash the neck of the flask. The solution should be clear
water to 100.0 mL. Each millilitre of the solution so prepared
and not greater than 20 mL in volume.
contains 10 μg of lead.
29. Procedure
A suitable prepared solution of this reagent, known as “Tiferron” or “Tiron,” is
supplied by the LaMotte Chemical Products Co., Baltimore, MD. 29.1 Pipet into a 50-mL Nessler tube 0.15 mL of HCl (1+2),
D 2363
2 mL of the buffer solution, and a volume of the standard lead METHOXYL CONTENT
solution containing the quantity of lead equivalent to the
30. Scope
specified heavy metals limit. Add water to make 40 mL and
30.1 This test method covers the determination of the
label as Solution A. Make sure that the final pH of these
methoxyl content of hydroxypropyl methylcellulose. Total
solutions is between 3 and 4. This can be tested by pH indicator
alkoxyl is first determined and the methoxyl content found by
paper or pH meter. For visual comparison make sure that the
subtracting the hydroxypropyl content from the total alkoxyl
optimum lead content is between 20 and 40 μg.
figure.
29.2 To the crucible containing the sulfated ash residue add
4 mL of HCl (1+2). Cover and carefully digest on a steam bath
31. Summary of Test Method
for 10 min. Uncover and slowly evaporate to dryness. Moisten
31.1 The hydroxypropyl methylcellulose is heated with a
the residue with 0.15 mL of HCl (1+2), 0.5 mL of hydroxy-
strong solution of hydriodic acid to form an alkyl iodide, which
lamine hydrochloride solution, and 10 mL of hot wa
...