ASTM D2363-79(2019)
(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:
Sections
Moisture
4 to 6
Ash (as Sulfate)
7 to 10
Chlorides (as NaCl)
11 to 14
Alkalinity (as Na2CO3)
15 to 18
Iron
19 to 24
Heavy Metals
25 to 29
Methoxyl Content
30 to 35
Hydroxypropoxyl Content
36 to 41
Viscosity
42 to 46
pH
47
Solids
48 to 51
Density
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see 33.5.1.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D2363 − 79 (Reapproved 2019)
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 D96 Test Method for Water and Sediment in Crude Oil by
Centrifuge Method (Field Procedure) (Withdrawn 2000)
1.1 These test methods cover the testing of hydroxypropyl
E70 Test Method for pH of Aqueous Solutions With the
methylcellulose.
Glass Electrode
1.2 The test procedures appear in the following order:
Sections 3. Purity of Reagents
3.1 Reagent grade chemicals shall be used in all tests.
Moisture 4 to 6
Ash (as Sulfate) 7 to 10
Unless otherwise indicated, it is intended that all reagents shall
Chlorides (as NaCl) 11 to 14
conform to the specifications of the Committee on Analytical
Alkalinity (as Na CO ) 15 to 18
2 3
Reagents of the American Chemical Society, where such
Iron 19 to 24
Heavy Metals 25 to 29
specifications are available. Other grades may be used, pro-
Methoxyl Content 30 to 35
vided it is first ascertained that the reagent is of sufficiently
Hydroxypropoxyl Content 36 to 41
high purity to permit its use without lessening the accuracy of
Viscosity 42 to 46
pH 47
the determination.
Solids 48 to 51
Density 52 to 56 3.2 Unless otherwise indicated, references to water shall be
understood to mean distilled water.
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
MOISTURE
only.
1.4 This standard does not purport to address all of the
4. Scope
safety concerns, if any, associated with its use. It is the
4.1 Thistestmethodcoversthedeterminationofthevolatile
responsibility of the user of this standard to establish appro-
content of hydroxypropyl methylcellulose and, by common
priate safety, health, and environmental practices and deter-
usage, designated moisture.
mine the applicability of regulatory limitations prior to use.
4.2 This international standard was developed in accor-
For a specific hazard statement, see 33.5.1.
dance with internationally recognized principles on standard-
1.5 This international standard was developed in accor-
ization established in the Decision on Principles for the
dance with internationally recognized principles on standard-
Development of International Standards, Guides and Recom-
ization established in the Decision on Principles for the
mendations issued by the World Trade Organization Technical
Development of International Standards, Guides and Recom-
Barriers to Trade (TBT) Committee.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Procedure
2. Referenced Documents 5.1 Transfer 2 to5gofthe sample weighed to the nearest
2 0.01 g to a tared dish (fitted with a lid) and dry for2hinan
2.1 ASTM Standards:
oven at 100 to 105°C with lid removed. Remove the dish from
the oven, cover with a lid, cool in a desiccator, and weigh.
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives. The last approved version of this historical standard is referenced on
Current edition approved Dec. 1, 2019. Published December 2019. Originally www.astm.org.
approved in 1965. Last previous edition approved in 2011 as D2363 – 79 (2011). ACS Reagent Chemicals, Specifications and Procedures for Reagents and
DOI: 10.1520/D2363-79R19. Standard-Grade Reference Materials, American Chemical Society, Washington,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2363 − 79 (2019)
6. Calculation sodiumchloride(NaCl)inhydroxypropylmethylcellulose.The
sample is dispersed and the chloride titrated volumetrically
6.1 Calculate the percent of moisture as follows:
with 0.100 N silver nitrate solution.
Moisture,% 5 A/B 3100 (1)
~ !
11.2 This international standard was developed in accor-
where:
dance with internationally recognized principles on standard-
A = mass loss on heating, and ization established in the Decision on Principles for the
B = sample used, g. Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
ASH—AS SULFATE
Barriers to Trade (TBT) Committee.
7. Scope
12. Reagents
7.1 Thistestmethodcoversthedeterminationoftheamount
12.1 Ferric Alum Indicator Solution—Add 100 g of ferric
of residue left from igniting a sample of hydroxypropyl
ammonium sulfate FeNH (SO ) ·12H O to 250 mL of water.
4 4 2 2
methylcellulose after being moistened with sulfuric acid.
Heat to boiling and add NHO (sp gr 1.42) slowly until the red
7.2 This international standard was developed in accor-
color is removed.This will usually require about 6 to 15 mLof
dance with internationally recognized principles on standard-
HNO . Filter the solution and store in a glass bottle.
ization established in the Decision on Principles for the
12.2 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
Development of International Standards, Guides and Recom-
(HNO ).
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
12.3 Potassium Thiocyanate Standard Solution (0.1 N)—
Dissolve 10 g of potassium thiocyanate (KCNS) in 1 L of
8. Reagents
water. By means of a pipet, measure 25 mL of 0.100 N silver
8.1 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
nitrate(AgNO )solutionintoa400-mLbeaker.Add100mLof
(HNO ).
water, 10 mL of HNO (sp gr 1.42), and 5 mL of ferric alum
8.2 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid indicator solution. Titrate with the KCNS solution, while
(H SO ). stirring, until a faint persistent red color is produced. Calculate
2 4
the normality, N, of the KCNS solution as follows:
9. Procedure
N 5 A/B 30.1 (3)
~ !
9.1 Weigh to the nearest 0.01 g about2gofthe sample
where:
(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
A = 0.100 N AgNO solution added, mL, and
2 4
the inside surface of the crucible. Place the crucible inside of a B = KCNS solution required for the titration, mL.
loosely fitting aluminum ring (approximately 32 mm (1 ⁄4 in.)
12.4 Silver Nitrate-Standard Solution (0.100 N)—Grind sil-
1 3
high, with 6.4-mm ( ⁄4-in.) sidewall, and 44-mm (1 ⁄4-in.)
ver nitrate (AgNO ) crystals fine enough to pass through a No.
inside diameter, cut from a piece of aluminum pipe) on a hot
20 (850-µm) sieve and then dry for2hat110°C. Prepare a
plate. Loosely cover with a crucible cover. Carefully char the
0.100 N solution by dissolving 16.989 g of dry AgNO in
hydroxypropyl methylcellulose until all the volatiles are re-
chloride-free water and diluting to 1 L in a volumetric flask.
moved.
9.2 Cool the crucible, add 1 ml of H SO and2mlofHNO
13. Procedure
2 4 3
so that it completely wets the charred residue. Cautiously heat
13.1 Weigh to the nearest 0.01 g about 1.0 g of the sample
to dense white fumes on a hot plate. Place the uncovered
(previously dried for ⁄2 h at 100 to 105°C) and transfer to a
crucible in a muffle furnace at 600°C and ignite until all the
500-mL, wide-mouth Erlenmeyer flask. Add 250 mL of hot
carbon is gone (for about 1 h). Transfer to a dessicator until
water and swirl for a few minutes; then cool to dissolve.
cool, then weigh. (Save the residue for the Heavy Metals
13.2 Add 5 mL of 0.100 N AgNO solution and 5 mL of
determination.) 3
ferric alum indicator solution, and back-titrate with 0.1 N
10. Calculation
KCNS solution to the first appearance of a faint pink color.
10.1 Calculate the percent of ash, C, as follows:
14. Calculation
C 5 A/B 3100 (2)
~ !
14.1 Calculate the percent of chlorides as NaCl as follows:
where:
Chlorides,% 5 ~@~AB 2 CD! 30.0585#/E! 3100 (4)
A = sulfated ash, g, and
B = sample used, g.
where:
A = AgNO solution added, mL,
CHLORIDES—AS SODIUM CHLORIDE
B = normality of the AgNO solution,
11. Scope C = KCNS solution required to back-titrate the excess
AgNO , mL,
11.1 This test method covers the determination of the total
D = normality of the KCNS solution, and
percent of chloride (bromide included if present) calculated as
D2363 − 79 (2019)
21. Reagents
E = sample used, g.
21.1 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
ALKALINITY—AS SODIUM CARBONATE
monium hydroxide (NH OH).
21.2 Buffer Solution—Dissolve 20 g of sodium bicarbonate
15. Scope
(NaHCO ) and 10 g of sodium carbonate (Na CO ) in water
3 2 3
15.1 This test method covers the determination of the total
and dilute to 1 L.
alkalinity of hydroxypropyl methylcellulose expressed as so-
21.3 Disodium-1,2-Dihydroxybenzene-3,5-Disulfonate
dium carbonate (Na CO ).
2 3
Solution—Prepare an aqueous solution containing 25 g/L.
15.2 This international standard was developed in accor-
21.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
dance with internationally recognized principles on standard-
chloric acid (HCl).
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
21.5 Hydrogen Peroxide (30%)—Concentrated hydrogen
mendations issued by the World Trade Organization Technical
peroxide (H O ).
2 2
Barriers to Trade (TBT) Committee.
21.6 Iron Standard Solution (0.0001 g Fe/ml)—Dissolve
0.01 g of iron powder containing not less than 99.9 % iron in
16. Reagents
HCl (sp gr 1.19). Oxidize the solution with bromine water and
16.1 Methyl Purple Indicator Solution.
expel the excess by boiling. Dilute to 1 Lin a volumetric flask.
16.2 Sulfuric Acid, Standard (0.01 N)—Prepare and stan-
21.7 Phenolphthalein Indicator Solution (1 g/100 mL)—
dardize a 0.01 N solution of sulfuric acid (H SO ).
2 4 Dissolve1gof phenolphthalein in 100 mL of ethanol (95 %).
21.8 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
17. Procedure
(H SO ).
2 4
17.1 Weigh to the nearest 0.01 g about 1.0 g of the sample
21.9 Sulfuric Acid (1+4)—Carefully mix 1 volume of
(previously dried for ⁄2 h at 100 to 105°C) and transfer to a
H SO (sp gr 1.84) with 4 volumes of water, adding the H SO
2 4 2 4
500-ml, widemouth Erlenmeyer flask. Add 250 mL of hot
gradually while mixing.
water and swirl for a few minutes; then cool to dissolve.
22. Preparation of Calibration Curve
17.2 Add 4 drops of methyl purple indicator solution and
titrate to the first faint pink color with 0.01 N H SO .
2 4 22.1 FollowingtheproceduregiveninSection23,andusing
varied amounts of the standard iron solution prepared in
18. Calculation
accordance with 21.6, prepare a calibration curve showing iron
18.1 Calculate the percent alkalinity as Na CO , S,as content in parts per million and the corresponding photometer
2 3
follows: readings.
S 5 @~AB 30.053!/C# 3100 (5)
23. Procedure
where: 23.1 Weigh to the nearest 0.01 g about2gofthe sample
(previously dried for ⁄2 h at 100 to 105°C). Transfer by means
A =H SO required for titration of the sample, mL,
2 4
of a funnel to a Kjeldahl flask. Place the flask at a 20° angle in
B = normality of the H SO , and
2 4
thefurnaceat500°Candheatuntilsomecharringofthesample
C = sample used, g.
has taken place. (Care must be taken not to char too much.)
IRON
Remove and allow to cool.
23.2 Add 3 mLof H SO to the flask. Place on the digestion
2 4
19. Scope
rack and digest. Cool and add H O dropwise until the solution
2 2
19.1 This test method covers the determination of total iron
is clear. Heat over a Meker burner to a volume of 2 mL. Cool,
content in samples of hydroxypropyl methylcellulose.The iron
and wash the sides of the flask with water. Add 3 drops of
is converted to ferric sulfate which reacts with the indicator to
phenolphthalein indicator solution. Add NH OH to a red end
form a pink color that can be quantitatively measured.
point. Wash the neck of the flask. The solution should be clear
19.2 This international standard was developed in accor-
and not greater than 20 mL in volume.
dance with internationally recognized principles on standard-
23.3 Add 2 mL of the color-forming solution described in
ization established in the Decision on Principles for the
21.3, and mix. Adjust pH to 7.0 and then dilute to mark with
Development of International Standards, Guides and Recom-
buffer. Transfer a small portion to an absorption cell and
mendations issued by the World Trade Organization Technical
determine the photometer reading at 480 nm.
Barriers to Trade (TBT) Committee.
23.4 Blank—Make a blank determination, using the same
amount of reagents and the same procedure as for the sample.
20. Apparatus
20.1 Photometer—Any photoelectric filter photometer or
24. Calculation
spectrophotometer suitable for measurements at 430 nm.
24.1 Read the iron content, in parts per million, directly
20.2 Kjeldahl Flasks—Calibrated to contain 50 mL, and from the calibration curve (Section 22). Subtract the parts per
made of heat- and chemical-resistant glass. million of iron due to iron in the blank.
D2363 − 79 (2019)
HEAVY METALS solution containing the quantity of lead equivalent to the
specified heavy metals limit. Add water to make 40 mL and
25. Scope
label as Solution A. Make sure that the final pH of these
solutionsisbetween3and4.ThiscanbetestedbypHindicator
25.1 This test method covers the determination of whether
or not the heavy metals content of hydroxypropyl methylcel- paper or pH meter. For visual comparison make sure that the
lulose is below a given level based on a lead standard. optimum lead content is between 20 and 40 µg.
25.2 This international standard was developed in accor-
29.2 To the crucible containing the sulfated ash residue add
dance with internationally recognized principles on stan
...
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