1、Designation: D5400 03 (Reapproved 2013)Standard Test Methods forHydroxypropylcellulose1This standard is issued under the fixed designation D5400; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i
2、n parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the testing of hydroxypropy-lcellulose.1.2 The test procedures appear in the following order:SectionsMoisture 4-9Visco
3、sity 10-16pH 17-21Residue on Ignition 22-28Hydroxypropoxy Content 29-361.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use
4、. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see 26.6.2. Referenced Documents2.1 ASTM Standards:2D3876 Test Method for Methoxyl and
5、Hydroxypropyl Sub-stitution in Cellulose Ether Products by Gas Chromatog-raphyE70 Test Method for pH of Aqueous Solutions With theGlass Electrode3. Reagents3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall confo
6、rm to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the
7、determination.3.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean distilled water.MOISTURE4. Scope4.1 This test method covers the determination of the volatilecontent of hydroxypropylcellulose.5. Significance and Use5.1 The results of this test are used for
8、calculating the totalsolids in the sample; and, by common usage, all materialsvolatile at this test temperature are designated as moisture.5.2 Moisture analysis (along with residue on ignition) is ameasure of the amount of active polymer in the material andmust be considered when determining the amo
9、unt of hydroxy-propylcellulose to use in various formulations.6. Apparatus6.1 Oven, gravity convection, capable of maintaining atemperature of 105 6 3C.6.2 Weighing Dish, glass or aluminum, with cover, 50 mmin diameter, 25 mm in height, or equivalent.6.3 Analytical Balance.7. Procedure7.1 Weigh abou
10、t5gofsample to the nearest 0.001 g in atared and covered weighing dish.7.2 Place it in an oven at 105 6 1C for 3 h with the coverremoved.7.3 Remove the dish from the oven, immediately replace thecover, cool in a desiccator, and weigh.1These test methods are under the jurisdiction of ASTM Committee D
11、01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved June 1, 2013. Published June 2013. Originallyapproved in 1993. Last previous edition approved in 2008 as D5400 03 (2008
12、).DOI: 10.1520/D5400-03R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemi
13、cal Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pha
14、rmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States18. Calculation8.1 Calculate the percent moisture, M, as follows:M 5 A/B! 3100 (1)where:A = mass loss on heating, g, andB = sample used, g
15、.8.2 Report the moisture content to the nearest 0.1 %.9. Precision and Bias9.1 PrecisionStatistical analysis of intralaboratory testresults on samples containing from 1 to 6 % moisture indicatesa precision of 60.2 % absolute at the 95 % confidence level.9.2 BiasNo justifiable statement on bias can b
16、e made asno suitable reference material is available as a standard.VISCOSITY10. Scope10.1 This test method is an arbitrary method of determiningthe viscosity of aqueous solutions of hydroxypropylcellulose inthe viscosity range of 10 to 16 000 cP/s at 25C.10.2 The concentration to be used for the tes
17、t shall beagreed upon between the purchaser and the seller. It shall besuch that the viscosity of the solution will fall within the rangeof this test.10.3 The results for the viscosity of hydroxypropylcelluloseby this test method will not necessarily check with results fromother types of instruments
18、 used for viscosity measurement.10.4 The determinations are run on a calculated dry basis;that is, the amount of hydroxypropylcellulose required for thedesired concentration on a dry basis is calculated from theknown moisture content.11. Significance and Use11.1 This test method is intended for refe
19、ree purposes. TheBrookfield4spindles and speeds given in Table 1 are recom-mended for this purpose, but slight deviations from Table 1may occasionally be found convenient for individual applica-tion.11.2 This test method determines the relative ability of thepolymer to thicken aqueous solutions and
20、is therefore related tothe concentration required in various formulations to achievethe desired finished product viscosity.12. Apparatus12.1 Viscometer, Brookfield Type.412.2 Container, glass bottle, 350-cm3(12-oz) approximately64 mm (212 in.) in outside diameter and 152 mm (6 in.) high.12.3 Mechani
21、cal 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 25C andcapable of maintaining that temperature to within 60.5C.13. Procedure13.1 Determine the moisture in accordance with Sections4-9.13.2 Calculate the
22、sample mass, S, in grams necessary tomake 250 g of test solution as follows:S 5A 3100100 2 B(2)where:A = desired dry mass of sample, g, andB = percent moisture in the weighed sample.13.3 Calculate the mass of water required, W, in grams asfollows:4Model LVF, available from Brookfield Engineering Lab
23、oratories, Inc.,Stoughton, MA has been found satisfactory for this purpose.TABLE 1 BrookfieldAViscometer Spindle and SpeedCombinationsViscosity Range,cPSpindleNumberSpeed,r/minScale Factor1080 1 60 100 120160 1 30 100 250400 2 60 100 5100800 2 30 100 104001600 3 60 100 208003200 3 30 100 4020008000
24、4 60 100 100400016 000 4 30 100 200ABrookfield Viscometer, Model LVF4.FIG. 1 Stainless Steel AgitatorD5400 03 (2013)2W 5 250 2 S (3)where:S = sample mass, g.13.4 Weigh the water into the glass bottle and place it on thestirrer, mixing at a speed sufficient to cause a vortex but not fastenough to spl
25、ash.13.5 Sprinkle the hydroxypropylcellulose sample into thewater slowly, to prevent lumping. Increase stirring speed toapproximately 900 6 100 r/min and stir until the sample iscompletely dissolved (1 to 2 h).13.6 Remove the glass bottle from the stirrer, cap the bottle,and place it in the constant
26、 temperature bath for 30 min or aslong as necessary to bring the solution to 25 6 0.5C.13.7 Remove the glass bottle from the water bath and invertit slowly 4 to 5 times, taking care to minimize the introductionof air bubbles.13.8 Measure the viscosity with the Brookfield viscometer,following the man
27、ufacturers operating instructions. Select theproper spindle and speed from Table 1. Allow the spindle torotate for 3 min before taking the reading. Use the spindleguard.NOTE 1If the room temperature is considerably greater or less than25C; the entire operation of stirring, standing, and measurement
28、shouldbe conducted with the glass bottle suspended in the constant temperaturebath.14. Calculation14.1 Calculate the viscosity, V, in centipoises as follows:V 5 r 3 f (4)where:r = scale reading andf = factor from Table 1.15. Report15.1 Report the following information:15.1.1 Results, as Brookfield v
29、iscosity at 25C,15.1.2 Solution concentration,15.1.3 Spindle used, and15.1.4 Speed used.16. Precision and Bias16.1 PrecisionStatistical analysis of interlaboratory testresults indicates a precision of 610 % at the 95 % confidencelevel.16.2 BiasNo justifiable statement on bias can be made asno suitab
30、le reference material is available as a standard.pH17. Scope17.1 This test method covers the determination of the pH ofaqueous solutions of hydroxypropylcellulose.18. Significance and Use18.1 This test method determines the relative acidity oralkalinity of aqueous solutions of hydroxypropylcellulose
31、. Thismust be taken into consideration when determining materialsof construction for equipment and packaging for handling andstoring these solutions. Also, pH may affect suitability forcertain end-use applications.19. Apparatus19.1 pH Meter, with glass electrodes.20. Procedure20.1 Determine the pH o
32、f the viscosity solution from 13.5,using a suitable pH meter that has been standardized accordingto Test Method E70.21. Precision and Bias21.1 PrecisionStatistical analysis of intralaboratory testresults on samples with pH values of 4.5 to 8.5 indicates aprecision of 65 % at the 95 % confidence leve
33、l.21.2 BiasNo justifiable statement on bias can be made asno suitable reference material is available as a standard.RESIDUE ON IGNITION22. Scope22.1 This test method covers the determination of theamount of residue left from igniting a sample of hydroxypro-pylcellulose after being moistened first wi
34、th sulfuric acid andthen with hydrofluoric acid.23. Significance and Use23.1 Excessive residue on ignition can affect solution clarityand film properties. The residue on ignition (along withmoisture) is a measure of the amount of active polymer in thematerial and must be considered when determining
35、the amountof hydroxypropylcellulose to use in various formulations.23.2 Commercially available hydroxypropylcellulose mostoften has up to 0.60 % silica added as an anti-caking agent.Therefore, a hydrofluoric acid ashing step is required toremove the silica.24. Apparatus24.1 Dishes, platinum, 75-mL c
36、apacity.24.2 Hot Plate.24.3 Muffle Furnace, capable of reaching 1000 6 25C.25. Reagents25.1 Sulfuric Acid (sp gr 1.84)concentrated sulfuric acid(H2SO4).25.2 Hydrofluoric Acid (48 %).26. Procedure26.1 Weigh, to the nearest 0.0001 g, about1gofhydroxy-propylcellulose into a tared platinum dish. Using a
37、 hot plate,heat the dish containing the sample (gently at first) until thesample is thoroughly charred. Cool the dish for severalminutes.D5400 03 (2013)326.2 Moisten the residue with about 1 mL of sulfuric acidand heat gently on the hot plate until white fumes are no longerevolved.26.3 Place the dis
38、h in a muffle furnace at 800 6 25C for 30min. Allow the dish to cool.26.4 Repeat 26.2 and 26.3. Cool in a desiccator. Weigh theresidue (R1).26.5 Moisten the residue with up to 1 mL of water andcarefully add about 5 mL of hydrofluoric acid, in smallportions. Evaporate to dryness on a hot plate in a f
39、ume hood.Allow the dish to cool.26.6 Carefully add about 5 mL of hydrofluoric acid and 0.5mL of sulfuric acid and evaporate to dryness on a hot plate ina fume hood. (WarningHydrofluoric acid is a poisonous andextremely hazardous acid because of its ability to cause severeburns that are not immediate
40、ly painful or visible. Use extremecare in handling.)26.7 Place the dish in a muffle furnace at 1000 6 25C for20 min. Allow the dish to cool in a desiccator. Weigh theresidue (R2).27. Calculations27.1 Calculate the percent residue on ignition, RI, as fol-lows:RI 5 R2/S! 3100 (5)where:R2= ash after ig
41、nition with hydrofluoric acid, g, andS = sample used, g.27.2 The percent silica content, Si, may be calculated asfollows:Si 5 R12 R2!/S 3100 (6)where:R1= ash after ignition with sulfuric acid, g,R2= ash after ignition with hydrofluoric acid, g, andS = sample used, g.28. Precision and Bias28.1 Precis
42、ionStatistical analysis of intralaboratory testresults on samples containing 0.00 to 0.30 % residue onignition indicates a precision of 610 % at the 95 % confidencelevel.28.2 BiasNo justifiable statement on bias can be made asno suitable reference material is available as a standard.HYDROXYPROPOXY C
43、ONTENT5,629. Scope29.1 This test method covers the determination of thehydroxypropoxy content of hydroxypropylcellulose.30. Summary of Test Method30.1 A sample of hydroxypropylcellulose is refluxed withaqueous chromic acid solution. The resulting acetic acid isdistilled and titrated with standard so
44、dium hydroxide solution.31. Significance and Use31.1 This test method determines the amount of substituentgroups added to the cellulose backbone. The level can affectsolution properties, rheology, solubility parameters, and filmproperties.31.2 Gas chromatographic procedures involving cleavage ofside
45、 groups with hydriodic acid (see Test Method D3876) arenot applicable for highly substituted hydroxypropylcellulosebecause the amount of hydriodic acid and the temperaturerequired to achieve complete reaction lead to side reactions thatrender the method non-quantitative.32. Apparatus32.1 Chromic Aci
46、d Oxidation Apparatus, as illustrated inFig. 2. The inlet for nitrogen and water in the reaction flask isa 1-mm capillary tip.32.2 Oil Bath, equipped with an electrical heating device sothe bath can be maintained at 155C.32.3 Analytical Balance, capable of weighing to 0.0001 g.33. Reagents33.1 Chrom
47、ium Trioxide Solution (30 %)Dissolve 30 g ofchromic trioxide (CrO3) in 70 ml of water.5References for the hydroxypropoxy determination are as follows: United StatesPharmacopeia XXII, General Chapter 421, “Hydroxypropoxy Determination,”1990, p. 1537, National Formulary XVII, “Monograph for Hydroxypro
48、pylCellulose,” 1990, p. 1938, United States Pharmacopeial Convention, Inc., 12601Twinbrook Parkway, Rockville, MD 20852.6Hercules Test Method No. K45-3, “Klucel Molecular Substitution,” HerculesTest Method No. M100-53, “Terminal Methyl Groups (Chromic Acid Oxidation),”available from Hercules, Inc. c
49、/o Aqualon Co., P.O. Box 271, Hopewell, VA23860-5245. Klucel is a registered trademark of Aqualon Co.D5400 03 (2013)433.2 NitrogenUse a nitrogen cylinder with suitable reduc-ing valve.33.3 Potassium Iodide (KI).33.4 Sodium Bicarbonate (NaHCO3)powder.33.5 Sodium Hydroxide Standard Solution (0.02 N), carbondioxide free.33.6 Sodium Thiosulfate Standard Solution (0.02 N).33.7 Sulfuric Acid Solution (10 %)Carefully add 60 mLofconcentrated sulfuric acid to 940 mL of water, slowly whilestirring.33.8 Phenolphthalein Indicator Solution, 1%.33.9 S
