ASTM D2363-79(2011)
(Test Method)Standard Test Methods for Hydroxypropyl Methylcellulose
Standard Test Methods for Hydroxypropyl Methylcellulose
ABSTRACT
These test methods cover the testing of hydroxypropyl methylcellulose. The test methods are as follows: moisture; ash; chlorides; alkalinity; iron; heavy metals; methoxyl content; hydroxyproproxyl content; viscosity; pH; solids; and density.
SCOPE
1.1 These test methods cover the testing of hydroxypropyl methylcellulose.
1.2 The test procedures appear in the following order:
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D2363 − 79 (Reapproved 2011)
Standard Test Methods for
Hydroxypropyl Methylcellulose
This standard is issued under the fixed designation D2363; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Purity of Reagents
3.1 Reagent grade chemicals shall be used in all tests.
1.1 These test methods cover the testing of hydroxypropyl
methylcellulose. Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical
1.2 The test procedures appear in the following order:
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
the determination.
Alkalinity (as Na CO ) 15 to 18
2 3
Iron 19 to 24
3.2 Unless otherwise indicated, references to water shall be
Heavy Metals 25 to 29
understood to mean distilled water.
Methoxyl Content 30 to 35
Hydroxypropoxyl Content 36 to 41
Viscosity 42 to 46 MOISTURE
pH 47
Solids 48 to 51 4. Scope
Density 52 to 56
4.1 Thistestmethodcoversthedeterminationofthevolatile
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.
5. Procedure
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 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
6.1 Calculate the percent of moisture as follows:
2. Referenced Documents
Moisture,% 5 ~A/B! 3100 (1)
2.1 ASTM Standards:
D96 Test Method for Water and Sediment in Crude Oil by
where:
Centrifuge Method (Field Procedure) (Withdrawn 2000)
A = mass loss on heating, and
E70 Test Method for pH of Aqueous Solutions With the
B = sample used, g.
Glass Electrode
ASH—AS SULFATE
7. Scope
These test methods are under the jurisdiction of ASTM Committee D01 on
7.1 Thistestmethodcoversthedeterminationoftheamount
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
of residue left from igniting a sample of hydroxypropyl
Current edition approved June 1, 2011. Published June 2011. Originally
methylcellulose after being moistened with sulfuric acid.
approved in 1965. Last previous edition approved in 2006 as D2363 – 79 (2006).
DOI: 10.1520/D2363-79R11.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Analar Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.astm.org. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2363 − 79 (2011)
8. Reagents stirring, until a faint persistent red color is produced. Calculate
the normality, N, of the KCNS solution as follows:
8.1 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
(HNO ). N 5 A/B 30.1 (3)
~ !
8.2 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
where:
(H SO ).
2 4
A = 0.100 N AgNO solution added, mL, and
B = KCNS solution required for the titration, mL.
9. Procedure
12.4 Silver Nitrate-Standard Solution (0.100 N)—Grind sil-
9.1 Weigh to the nearest 0.01 g about2gofthe sample
ver nitrate (AgNO ) crystals fine enough to pass through a No.
(previously dried for ⁄2 h at 105°C) into a tared Coors No. 1,
20 (850-µm) sieve and then dry for2hat110°C. Prepare a
high-form, porcelain crucible. Add 5 drops of H SO around
2 4 0.100 N solution by dissolving 16.989 g of dry AgNO in
the inside surface of the crucible. Place the crucible inside of a
chloride-free water and diluting to 1 L in a volumetric flask.
loosely fitting aluminum ring (approximately 32 mm (1 ⁄4 in.)
1 3
high, with 6.4-mm ( ⁄4-in.) sidewall, and 44-mm (1 ⁄4-in.)
13. Procedure
inside diameter, cut from a piece of aluminum pipe) on a hot
13.1 Weigh to the nearest 0.01 g about 1.0 g of the sample
plate. Loosely cover with a crucible cover. Carefully char the
(previously dried for ⁄2 h at 100 to 105°C) and transfer to a
hydroxypropyl methylcellulose until all the volatiles are re-
500-mL, wide-mouth Erlenmeyer flask. Add 250 mL of hot
moved.
water and swirl for a few minutes; then cool to dissolve.
9.2 Cool the crucible, add 1 ml of H SO and2mlofHNO
2 4 3
13.2 Add 5 mL of 0.100 N AgNO solution and 5 mL of
so that it completely wets the charred residue. Cautiously heat
ferric alum indicator solution, and back-titrate with 0.1 N
to dense white fumes on a hot plate. Place the uncovered
KCNS solution to the first appearance of a faint pink color.
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
14. Calculation
cool, then weigh. (Save the residue for the Heavy Metals
14.1 Calculate the percent of chlorides as NaCl as follows:
determination.)
Chlorides,% 5 ~@~AB 2 CD! 30.0585#/E! 3100 (4)
10. Calculation
where:
10.1 Calculate the percent of ash, C, as follows:
A = AgNO solution added, mL,
B = normality of the AgNO solution,
C 5 A/B 3100 (2) 3
~ !
C = KCNS solution required to back-titrate the excess
where:
AgNO , mL,
A = sulfated ash, g, and D = normality of the KCNS solution, and
B = sample used, g.
E = sample used, g.
CHLORIDES—AS SODIUM CHLORIDE ALKALINITY—AS SODIUM CARBONATE
15. Scope
11. Scope
15.1 This test method covers the determination of the total
11.1 This test method covers the determination of the total
alkalinity of hydroxypropyl methylcellulose expressed as so-
percent of chloride (bromide included if present) calculated as
dium carbonate (Na CO ).
sodiumchloride(NaCl)inhydroxypropylmethylcellulose.The 2 3
sample is dispersed and the chloride titrated volumetrically
16. Reagents
with 0.100 N silver nitrate solution.
16.1 Methyl Purple Indicator Solution.
12. Reagents
16.2 Sulfuric Acid, Standard (0.01 N)—Prepare and stan-
12.1 Ferric Alum Indicator Solution—Add 100 g of ferric dardize a 0.01 N solution of sulfuric acid (H SO ).
2 4
ammonium sulfate FeNH (SO ) ·12H O to 250 mL of water.
4 4 2 2
17. Procedure
Heat to boiling and add NHO (sp gr 1.42) slowly until the red
color is removed.This will usually require about 6 to 15 mLof
17.1 Weigh to the nearest 0.01 g about 1.0 g of the sample
HNO . Filter the solution and store in a glass bottle.
(previously dried for ⁄2 h at 100 to 105°C) and transfer to a
500-ml, widemouth Erlenmeyer flask. Add 250 mL of hot
12.2 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
water and swirl for a few minutes; then cool to dissolve.
(HNO ).
17.2 Add 4 drops of methyl purple indicator solution and
12.3 Potassium Thiocyanate Standard Solution (0.1 N)—
titrate to the first faint pink color with 0.01 N H SO .
Dissolve 10 g of potassium thiocyanate (KCNS) in 1 L of 2 4
water. By means of a pipet, measure 25 mL of 0.100 N silver
18. Calculation
nitrate(AgNO )solutionintoa400-mLbeaker.Add100mLof
water, 10 mL of HNO (sp gr 1.42), and 5 mL of ferric alum 18.1 Calculate the percent alkalinity as Na CO , S,as
3 2 3
indicator solution. Titrate with the KCNS solution, while follows:
D2363 − 79 (2011)
S 5 AB 30.053 /C 3100 (5) thefurnaceat500°Candheatuntilsomecharringofthesample
@~ ! #
has taken place. (Care must be taken not to char too much.)
where:
Remove and allow to cool.
A =H SO required for titration of the sample, mL,
2 4
23.2 Add 3 mLof H SO to the flask. Place on the digestion
B = normality of the H SO , and 2 4
2 4
rack and digest. Cool and add H O dropwise until the solution
C = sample used, g. 2 2
is clear. Heat over a Meker burner to a volume of 2 mL. Cool,
IRON
and wash the sides of the flask with water. Add 3 drops of
phenolphthalein indicator solution. Add NH OH to a red end
19. Scope
point. Wash the neck of the flask. The solution should be clear
19.1 This test method covers the determination of total iron
and not greater than 20 mL in volume.
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.
20.2 Kjeldahl Flasks—Calibrated to contain 50 mL, and
24. Calculation
made of heat- and chemical-resistant glass.
24.1 Read the iron content, in parts per million, directly
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-
monium hydroxide (NH OH).
HEAVY METALS
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.
21.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
26. Summary of Test Method
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 ).
amount of lead is prepared, and the heavy metals content is
2 2
determined qualitatively by comparing the sample to the
21.6 Iron Standard Solution (0.0001 g Fe/ml)—Dissolve
standard.
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. Apparatus
expel the excess by boiling. Dilute to 1 Lin a volumetric flask.
27.1 Nessler Tubes, 50-mL.
21.7 Phenolphthalein Indicator Solution (1 g/100 mL)—
27.2 Volumetric Flasks, 50-mL.
Dissolve1gof phenolphthalein in 100 mL of ethanol (95 %).
21.8 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
28. Reagents
(H SO ).
2 4
28.1 Acetic Acid—Glacial acetic acid.
21.9 Sulfuric Acid (1+4)—Carefully mix 1 volume of
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
2 4 2 4
monium hydroxide (NH OH).
gradually while mixing. 4
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.
22.1 FollowingtheproceduregiveninSection23,andusing
28.4 Buffer Solution—Dissolve 60 mL of acetic acid in
varied amounts of the standard iron solution prepared in
about 500 mL of water, add 10 mL of NH OH, and dilute to 1
accordance with 21.6, prepare a calibration curve showing iron
L.
content in parts per million and the corresponding photometer
28.5 HydrochloricAcid (1+2)—Dilute 1 volume of concen-
readings.
trated hydrochloric acid (HCl, sp gr 1.19) with 2 volumes of
23. Procedure water.
23.1 Weigh to the nearest 0.01 g about2gofthe sample 28.6 HydrogenSulfideTS—Saturate a convenient volume of
(previously dried for ⁄2 h at 100 to 105°C). Transfer by means water with hydrogen sulfide (H S) in a narrow-neck, glass-
of a funnel to a Kjeldahl flask. Place the flask at a 20° angle in stoppered, amber bottle. This solution must be made fresh.
D2363 − 79 (2011)
28.7 Hydroxylamine Hydrochloride Solution (200 g/L)— 32. Apparatus
Dissolve 20 g of hydroxylamine hydrochloride (NH OH·HCl)
32.1 Distillation Apparatus, as illustrated in Fig. 1, consist-
in 100 mL of water.
ing of a boiling flask with a side arm for admission of carbon
28.8 Lead Nitrate Stock Solution—Dissolve 159.8 mg of dioxide or nitrogen, an air condenser with a trap, and a
lead nitrate (Pb(NO ) ) in 100 mLof water containing 1 mLof receiver.
3 2
HNO (sp gr 1.42). Dilute with water to 1000.0 mL and mix.
32.2 Oil Bath, equipped with a heating device, preferably
This solution should be prepared and stored in glass containers
electrical, so that the bath can be maintained at 145 to 150°C.
that are free from lead salts.
33. Reagents
28.9 Lead Standard Solution (1 mL=1 µg Pb)—Dilute 10
33.1 Bromine Solution—Dissolve 5 mL of bromine in 145
mLoftheleadnitratestocksolution,accuratelymeasured,with
mL of the potassium acetate solution. Prepare the bromine
water to 100.0 mL. Each millilitre of the solution so prepared
solution fresh daily in a hood to remove bromine vapors.
contains 10 µg of lead.
33.2 Carbon Dioxide—This may be obtained by the inter-
29. Procedure
action of marble and hydrochloric acid (HCl, 1+1) in a Kipp
29.1 Pipet into a 50-mLNessler tube 0.15 mLof HCl (1+2), generator or preferably from a cylinder of the gas equipped
2 mL of the buffer solution, and a volume of the standard lead
withasuitableneedlevalve.Thecarbondioxide(CO )shallbe
solution containing the quantity of lead equivalent to the passed through a bubble counter and a dry trap, and then
specified heavy metals limit. Add water to make 40 mL and
through a pressure regulator consisting of a glass tee
...
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