ASTM D2363-79(2000)e1
(Test Method)Standard Test Methods for Hydroxypropyl Methylcellulose
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
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e1
Designation:D2363–79 (Reapproved 2000)
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 November 2000.
1. Scope 3. Purity of Reagents
1.1 These test methods cover the testing of hydroxypropyl 3.1 Reagent grade chemicals shall be used in all tests.
methylcellulose. Unless otherwise indicated, it is intended that all reagents shall
1.2 The test procedures appear in the following order: conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
Sections
specifications are available. Other grades may be used, pro-
Moisture 4 to 6
vided it is first ascertained that the reagent is of sufficiently
Ash (as Sulfate) 7 to 10
high purity to permit its use without lessening the accuracy of
Chlorides (as NaCl) 11 to 14
Alkalinity (as Na CO ) 15to18
2 3
the determination.
Iron 19to24
3.2 Unless otherwise indicated, references to water shall be
Heavy Metals 25 to 29
Methoxyl Content 30 to 35 understood to mean distilled water.
Hydroxypropoxyl Content 36 to 41
Viscosity 42 to 46
MOISTURE
pH 47
Solids 48to51
4. Scope
Density 52 to 56
4.1 This test method covers the determination of the volatile
1.3 The values stated in SI units are to be regarded as the
content of hydroxypropyl methylcellulose and, by common
standard. The values given in parentheses are for information
usage, designated moisture.
only.
1.4 This standard does not purport to address all of the
5. Procedure
safety concerns, if any, associated with its use. It is the
5.1 Transfer 2 to5gofthe sample weighed to the nearest
responsibility of the user of this standard to establish appro-
0.01 g to a tared dish (fitted with a lid) and dry for2hinan
priate safety and health practices and determine the applica-
oven at 100 to 105°C with lid removed. Remove the dish from
bility of regulatory limitations prior to use. For a specific
the oven, cover with a lid, cool in a desiccator, and weigh.
hazard statement, see 33.5.1.
6. Calculation
2. Referenced Documents
6.1 Calculate the percent of moisture as follows:
2.1 ASTM Standards:
Moisture, % 5 ~A/B! 3 100 (1)
D 96 Test Methods for Water and Sediment in Crude Oil by
Centrifuge Method (Field Procedure)
where:
E 70 Test Method for pH of Aqueous Solutions With the
A = mass loss on heating, and
Glass Electrode
B = sample used, g.
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct Reagent Chemicals, American Chemical Society Specifications, American
responsibility 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. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.05. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2363
ASH—AS SULFATE water. By means of a pipet, measure 25 mL of 0.100 N silver
nitrate(AgNO )solutionintoa400-mLbeaker.Add100mLof
7. Scope
water, 10 mL of HNO (sp gr 1.42), and 5 mL of ferric alum
7.1 This test method covers the determination of the amount indicator solution. Titrate with the KCNS solution, while
stirring, until a faint persistent red color is produced. Calculate
of residue left from igniting a sample of hydroxypropyl
methylcellulose after being moistened with sulfuric acid. the normality, N, of the KCNS solution as follows:
N 5 A/B 3 0.1 (3)
~ !
8. Reagents
where:
8.1 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
A = 0.100 N AgNO solution added, mL, and
(HNO ). 3
B = KCNS solution required for the titration, mL.
8.2 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
12.4 Silver Nitrate-Standard Solution (0.100 N)—Grind
(H SO ).
2 4
silver nitrate (AgNO ) crystals fine enough to pass through a
9. Procedure No. 20 (850-µm) sieve and then dry for2hat110°C. Prepare
a 0.100 N solution by dissolving 16.989 g of dry AgNO in
9.1 Weigh to the nearest 0.01 g about2gofthe sample
1 chloride-free water and diluting to 1 L in a volumetric flask.
(previously dried for ⁄2 h at 105°C) into a tared Coors No. 1,
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
13.1 Weigh to the nearest 0.01 g about 1.0 g of the sample
loosely fitting aluminum ring (approximately 32 mm (1 ⁄4 in.)
(previously dried for ⁄2h at 100 to 105°C) and transfer to a
1 3
high, with 6.4-mm ( ⁄4-in.) sidewall, and 44-mm (1 ⁄4-in.)
500-mL, wide-mouth Erlenmeyer flask. Add 250 mL of hot
inside diameter, cut from a piece of aluminum pipe) on a hot
water and swirl for a few minutes; then cool to dissolve.
plate. Loosely cover with a crucible cover. Carefully char the
13.2 Add 5 mL of 0.100 N AgNO solution and 5 mL of
hydroxypropyl methylcellulose until all the volatiles are re-
ferric alum indicator solution, and back-titrate with 0.1 N
moved.
KCNS solution to the first appearance of a faint pink color.
9.2 Coolthecrucible,add1mlofH SO and2mlofHNO
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
Chlorides, % 5 ~@~AB 2CD! 3 0.0585#/E! 3 100 (4)
carbon is gone (for about 1 h). Transfer to a dessicator until
cool, then weigh. (Save the residue for the Heavy Metals
where:
determination.)
A = AgNO solution added, mL,
B = normality of the AgNO solution,
10. Calculation
C = KCNS solution required to back-titrate the excess
10.1 Calculate the percent of ash, C, as follows: AgNO , mL,
D = normality of the KCNS solution, and
C 5 ~A/B! 3 100 (2)
E = sample used, g.
where:
ALKALINITY—AS SODIUM CARBONATE
A = sulfated ash, g, and
B = sample used, g.
15. Scope
15.1 This test method covers the determination of the total
CHLORIDES—AS SODIUM CHLORIDE
alkalinity of hydroxypropyl methylcellulose expressed as so-
dium carbonate (Na CO ).
11. Scope
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.
sodiumchloride(NaCl)inhydroxypropylmethylcellulose.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 ).
2 4
with 0.100 N silver nitrate solution.
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 1
(previously dried for ⁄2h 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 mLof
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
18. Calculation
(HNO ).
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:
D2363
S 5 @~AB 3 0.053!/C# 3 100 (5) 23.2 Add 3 mLof H SO to the flask. Place on the digestion
2 4
rackanddigest.CoolandaddH O dropwiseuntilthesolution
2 2
where:
is clear. Heat over a Meker burner to a volume of 2 mL. Cool,
A =H SO required for titration of the sample, mL,
2 4
and wash the sides of the flask with water. Add 3 drops of
B = normality of the H SO , and
2 4
phenolphthalein indicator solution. Add NH OH to a red end
C = sample used, g.
point. Wash the neck of the flask. The solution should be clear
and not greater than 20 mL in volume.
IRON
23.3 Add 2 mL of the color-forming solution described in
21.3, and mix. Adjust pH to 7.0 and then dilute to mark with
19. Scope
buffer. Transfer a small portion to an absorption cell and
19.1 This test method covers the determination of total iron
determine the photometer reading at 480 nm.
content in samples of hydroxypropyl methylcellulose.The iron
23.4 Blank—Make a blank determination, using the same
is converted to ferric sulfate which reacts with the indicator to
amount of reagents and the same procedure as for the sample.
form a pink color that can be quantitatively measured.
24. Calculation
20. Apparatus
24.1 Read the iron content, in parts per million, directly
20.1 Photometer—Any photoelectric filter photometer or
from the calibration curve (Section 22). Subtract the parts per
spectrophotometer suitable for measurements at 430 nm.
million of iron due to iron in the blank.
20.2 Kjeldahl Flasks—Calibrated to contain 50 mL, and
made of heat- and chemical-resistant glass.
HEAVY METALS
21. Reagents
25. Scope
21.1 AmmoniumHydroxide(spgr0.90)—Concentrated am-
25.1 This test method covers the determination of whether
monium hydroxide (NH OH).
or not the heavy metals content of hydroxypropyl methylcel-
21.2 Buffer Solution—Dissolve 20 g of sodium bicarbonate
lulose is below a given level based on a lead standard.
(NaHCO ) and 10 g of sodium carbonate (Na CO ) in water
3 2 3
and dilute to 1 L.
26. Summary of Test Method
21.3 Disodium-1,2-Dihydroxybenzene-3,5-Disulfonate
26.1 The ash residue from the sulfated ash test is digested
Solution—Prepare an aqueous solution containing 25 g/L.
with dilute hydrochloric acid. A standard containing a known
21.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
amount of lead is prepared, and the heavy metals content is
chloric acid (HCl).
determined qualitatively by comparing the sample to the
21.5 Hydrogen Peroxide (30%)—Concentrated hydrogen
standard.
peroxide (H O ).
2 2
21.6 Iron Standard Solution (0.0001 g Fe/ml)—Dissolve
27. Apparatus
0.01 g of iron powder containing not less than 99.9 % iron in
HCl (sp gr 1.19). Oxidize the solution with bromine water and 27.1 Nessler Tubes, 50-mL.
expel the excess by boiling. Dilute to 1 Lin a volumetric flask. 27.2 Volumetric Flasks, 50-mL.
21.7 Phenolphthalein Indicator Solution (1 g/100 mL)—
Dissolve1gof phenolphthalein in 100 mL of ethanol (95 %). 28. Reagents
21.8 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
28.1 Acetic Acid—Glacial acetic acid.
(H SO ).
2 4
28.2 AmmoniumHydroxide(spgr0.90)—Concentrated am-
21.9 SulfuricAcid(1+4)—Carefullymix1volumeofH SO
2 monium hydroxide (NH OH).
4 (sp gr 1.84) with 4 volumes of water, adding the H SO
2 4 28.3 Ammonium Hydroxide (2+3)—Dilute 400 mL of
gradually while mixing.
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. Preparation of Calibration Curve
about 500 mL of water, add 10 mL of NH OH, and dilute to 1
22.1 FollowingtheproceduregiveninSection23,andusing
L.
varied amounts of the standard iron solution prepared in
28.5 HydrochloricAcid (1+2)—Dilute 1 volume of concen-
accordance with 21.6, prepare a calibration curve showing iron
trated hydrochloric acid (HCl, sp gr 1.19) with 2 volumes of
content in parts per million and the corresponding photometer
water.
readings.
28.6 HydrogenSulfideTS—Saturateaconvenientvolumeof
water with hydrogen sulfide (H S) in a narrow-neck, glass-
23. Procedure
stoppered, amber bottle. This solution must be made fresh.
23.1 Weigh to the nearest 0.01 g about2gofthe sample 28.7 Hydroxylamine Hydrochloride Solution (200 g/L)—
(previously dried for ⁄2 h at 100 to 105°C). Transfer by means Dissolve 20 g of hydroxylamine hydrochloride (NH OH·HCl)
of a funnel to a Kjeldahl flask. Place the flask at a 20° angle in in 100 mL of water.
thefurnaceat500°Candheatuntilsomecharringofthesample 28.8 Lead Nitrate Stock Solution—Dissolve 159.8 mg of
has taken place. (Care must be taken not to char too much.) lead nitrate (Pb(NO ) ) in 100 mLof water containing 1 mLof
3 2
Remove and allow to cool. HNO (sp gr 1.42). Dilute with water to 1000.0 mL and mix.
D2363
This solution should be prepared and stored in glass containers 33. Reagents
that are free from lead salts.
33.1 Bromine Solution—Dissolve 5 mL of bromine in 145
28.9 Lead Standard Solution (1 mL=1 µg Pb)—Dilute 10
mL of the potassium acetate solution. Prepare the bromine
mLoftheleadnitratestocksolution,accuratelymeasured,with
solution fresh daily in a hood to remove bromine vapors.
water to 100.0 mL. Each millilitre of the solution so prepared
33.2 Carbon Dioxide—This may be obtained by the inter-
contains 10 µg of lead.
action of marble and hydrochloric acid (HCl, 1+1) in a Kipp
generator or preferably from a cylinder of the gas equipped
29. Procedure
withasuitableneedlevalve.Thecarbondioxide(CO )shallbe
29.1 Pipet into a 50-mLNessler tube 0.15 mLof HCl (1+2),
passed through a bubble counter and a dry trap, and then
2 mL of the buffer solution, and a volume of the standard lead
through a pressure regulator consisting of a glass tee whose
solution containing the quantity of lead equivalent to the
vertical arm extends almost to the bottom of a 10-in. (254-mm)
specified heavy metals limit. Add water to make 40 mL and
column of water. A screw clamp shall be attached to the
label as Solution A. Make sure that the final pH of these
thin-walled rubber tubing connecting the horizontal arm of the
solutionsisbetween3and4.ThiscanbetestedbypHindicator
tee with the boiling flask. This arrangement permits regulation
paper or pH meter. For visual comparison make sure that the
of the flow of gas and allows any excess gas to escape.
optimum lead content is between 20 and 40 µg.
Nitrogen may be used in place of CO .
29.2 To the crucible containing the sulfated ash residue add
33.3 Formic Acid (90%).
...
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