1、Designation: D 5400 03Standard Test Methods forHydroxypropylcellulose1This standard is issued under the fixed designation D 5400; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses in
2、dicates the year of last reapproval. Asuperscript epsilon (e) 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 to 9Viscosity 10 to 1
3、6pH 17 to 21Residue on Ignition 22 to 28Hydroxypropoxy Content 29 to 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:2D 3876 Test Method for Methoxyl and
5、 HydroxypropylSubstitution in Cellulose Ether Products by Gas Chroma-tographyE 70 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 hydrox-ypropylcellulose 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.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of
11、Subcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved Dec. 1, 2003. Published January 2004. Originallyapproved in 1993. Last previous edition approved in 1993 as D 5400 93 (1997).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custom
12、er Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notli
13、sted 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. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, We
14、st Conshohocken, PA 19428-2959, United States.7.3 Remove the dish from the oven, immediately replace thecover, cool in a desiccator, and weigh.8. Calculation8.1 Calculate the percent moisture, M, as follows:M 5 A/B! 3 100 (1)where:A = mass loss on heating, g, andB = sample used, g.8.2 Report the moi
15、sture 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 be made asno suitabl
16、e 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 test shall beagreed up
17、on 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 used for viscosity
18、 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 referee purposes. TheBr
19、ookfield4spindles 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 is therefore relate
20、d 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 Mechanical Stirrer, agitat
21、or 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 6 0.5C.13. Procedure13.1 Determine the moisture in accordance with Sections4-9.13.2 Calculate the sample mass, S, in
22、 grams necessary tomake 250 g of test solution as follows:S 5A 3 100100 2 B(2)where:A = desired dry mass of sample, g, andB = percent moisture in the weighed sample.4Model LVF, available from Brookfield Engineering Laboratories, Inc., Stough-ton, MA has been found satisfactory for this purpose.TABLE
23、 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 4 60 100 100400016 000 4 30 100 200ABrookfield Viscometer, Model LVF4.FIG. 1 Sta
24、inless Steel AgitatorD540003213.3 Calculate the mass of water required, W, in grams asfollows:W 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 splash.13.5 Sprinkle the h
25、ydroxypropylcellulose 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 temperature bath for 3
26、0 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 manufacturers operating in
27、structions. 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 shouldbe conducted with
28、 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 viscosity at 25C,15.1.2
29、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 suitable reference material i
30、s 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. Thismust be taken int
31、o 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 of the viscosity solutio
32、n from 13.5,using a suitable pH meter that has been standardized accordingto Test Method E 70.21. 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 level.21.2 BiasNo justifia
33、ble 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 with sulfuric acid andth
34、en 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 the amountof hydroxypr
35、opylcellulose 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 capacity.24.2 Hot Plate
36、.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, about1gofhydrox-ypropylcellulose into a tared platinum dish. Using a hot plate,heat the d
37、ish containing the sample (gently at first) until thesample is thoroughly charred. Cool the dish for severalminutes.26.2 Moisten the residue with about 1 mL of sulfuric acidand heat gently on the hot plate until white fumes are no longerevolved.D540003326.3 Place the dish in a muffle furnace at 800
38、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 fume hood.Allow the dish to co
39、ol.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 immediately painful or visible. Use ex
40、tremecare 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! 3 100 (5)where:R2= ash after ignition with hydrofluoric aci
41、d, g, andS = sample used, g.27.2 The percent silica content, Si, may be calculated asfollows:Si 5 R12 R2!/S 3 100 (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 PrecisionStatistical analysis of
42、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 CONTENT5,629. Scope29.1 This
43、 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 sodium hydroxide solution.31.
44、 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 groups with hydriodic acid
45、 (see Test Method D 3876) 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 Acid Oxidation Apparatus, as
46、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 Chromium Trioxide Solution (30
47、%)Dissolve 30 g ofchromic trioxide (CrO3) in 70 ml of water.33.2 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 Solut
48、ion (0.02 N).5References for the hydroxypropoxy determination are as follows: United StatesPharmacopeia XXII, General Chapter 421 hydroxypropylcellulose;moisture; pH; residue on ignition; viscosityASTM International takes no position respecting the validity of any patent rights asserted in connectio
49、n with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Hea
