1、Designation: D5400 03 (Reapproved 2013)D5400 15Standard 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
2、number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 These test methods cover the testing of hydroxypropylcellulose.1.2 The test procedures appear in the following order:SectionsMoi
3、sture 4 9Viscosity 10 16pH 17 21Residue on Ignition 22 28Hydroxypropoxy Content 29 361.3 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, associ
4、ated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see 26.6.2. Referenced Documents2.1 ASTM Standards:2D3876 Test Method fo
5、r Methoxyl and Hydroxypropyl Substitution in Cellulose Ether Products by Gas ChromatographyE70 Test Method for pH of Aqueous Solutions With the Glass Electrode3. Reagents3.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreage
6、nts shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the
7、 accuracy of the determination.3.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean distilled water.MOISTURE4. Scope4.1 This test method covers the determination of the volatile content of hydroxypropylcellulose.5. Significance and Use5.1 The results of this
8、 test are used for calculating the total solids in the sample; and, by common usage, all materials volatileat this test temperature are designated as moisture.5.2 Moisture analysis (along with residue on ignition) is a measure of the amount of active polymer in the material and mustbe considered whe
9、n determining the amount of hydroxypropylcellulose to use in various formulations.1 These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility ofSubcommittee D01.36 on Cellulose and Cellulose Deriva
10、tives.Current edition approved June 1, 2013Dec. 1, 2015. Published June 2013January 2016. Originally approved in 1993. Last previous edition approved in 20082013 asD5400 03 (2008).(2013). DOI: 10.1520/D5400-03R13.10.1520/D5400-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, o
11、r contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page on the ASTM website.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions
12、on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.This document is not an ASTM standa
13、rd and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases
14、only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Apparatus6.1 Ov
15、en, gravity convection, capable of maintaining a temperature of 105 6 3C.6.2 Weighing Dish, glass or aluminum, with cover, 50 mm in diameter, 25 mm in height, or equivalent.6.3 Analytical Balance.7. Procedure7.1 Weigh about 5 g of sample to the nearest 0.001 g in a tared and covered weighing dish.7.
16、2 Place it in an oven at 105 6 1C for 3 h with the cover removed.7.3 Remove the dish from the oven, immediately replace the cover, cool in a desiccator, and weigh.8. Calculation8.1 Calculate the percent moisture, M, as follows:M 5A/B! 3100 (1)where:A = mass loss on heating, g, andB = sample used, g.
17、8.2 Report the moisture content to the nearest 0.1 %.9. Precision and Bias9.1 PrecisionStatistical analysis of intralaboratory test results on samples containing from 1 to 6 % moisture indicates aprecision of 60.2 % absolute at the 95 % confidence level.9.2 BiasNo justifiable statement on bias can b
18、e made as no suitable reference material is available as a standard.VISCOSITY10. Scope10.1 This test method is an arbitrary method of determining the viscosity of aqueous solutions of hydroxypropylcellulose in theviscosity range of 10 to 16 000 cP/s mPa s (cP) at 25C.10.2 The concentration to be use
19、d for the test shall be agreed upon between the purchaser and the seller. It shall be such thatthe viscosity of the solution will fall within the range of this test.TABLE 1 BrookfieldA Viscometer Spindle and SpeedCombinationsViscosity Range,cPSpindleNumberSpeed,r/min ScaleFactor1080 1 60 100 120160
20、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 200TABLE 1 Cylindrical Rotational Elements and Speeds(see Fig. 1)Viscosity Range,(mPas)Diameter (D)(mm)Length (L)(mm)Speed(rmin)TorqueScaleMultiplier10 to 80 19 65 60 120 to 160
21、 19 65 30 250 to 400 10 54 60 5100 to 800 10 54 30 10400 to 1600 5.9 43 60 20800 to 3200 5.9 43 30 402000 to 8000 3.2 31 60 1004000 to 16 000 3.2 31 30 200A Brookfield Viscometer, Model LVF4.D5400 15210.3 The results for the viscosity of hydroxypropylcellulose by this test method will not necessaril
22、y checkagree with resultsfrom other types of instruments used for viscosity measurement.10.4 The determinations are run on a calculated dry basis; that is, the amount of hydroxypropylcellulose required for the desiredconcentration on a dry basis is calculated from the known moisture content.11. Sign
23、ificance and Use11.1 This test method is intended for referee purposes. The BrookfieldThe rotational spindleselements and speeds given in Table1 are recommended for this purpose, but slight purpose. Slight deviations from Table 1 may occasionally be found convenient foran individual application.11.2
24、 This test method determines the relative ability of the polymer to thicken aqueous solutions and is therefore related to theconcentration required in various formulations to achieve the desired finished product viscosity.12. Apparatus12.1 Viscometer, Brookfield Type.412.1 Container, Viscometer, Rot
25、ationalglass bottle, 350-cmThe essential instrumentation3 (12-oz) approximately 64 mm(2required providing the minimum rotational12 in.) in outside diameter and 152 mm (6 in.) high.viscometer analytical capabilitiesfor this method include:12.1.1 Adrive motor, to apply a unidirectional displacement to
26、 the specimen at a rate from 0.5 to 60 rev/min constant to within61 %.12.1.2 A force sensor to measure the torque developed by the specimen.12.1.3 A coupling shaft or other means to transmit the rotational displacement from the motor to the specimen.NOTE 1It is helpful to have a mark on the shaft to
27、 indicate the appropriate level of the specimen.12.1.4 A rotational element, spindle or tool to fix the specimen between the drive shaft and a stationary position.NOTE 2The rotational element shall be of the immersion type. This standard is not intended for cone-and-plate or parallel plate type visc
28、ometers.NOTE 3Each rotational element typically covers a range of about two decades of viscosity. The rotational element is selected so that the measuredFIG. 1 Cylindrical Rotational Elements and SpeedsD5400 153viscosity is between 15 and 95 % of the range of the rotational element.12.1.5 A guard to
29、 protect the rotational element from mechanical damage.12.1.6 A temperature sensor to provide an indication of the specimen temperature of the range of 20 to 30C to within 0.1C.12.1.7 Adata collection device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or
30、 both.The minimum output signals required for rotational viscometry are torque, rotational speed, temperature, and time.12.1.8 A stand, to support, level, and adjust the height of the drive motor, shaft, and rotational element.12.1.9 Container, glass bottle, 350-cm3 (12-oz) approximately 64 mm (212
31、in.) in outside diameter and 152 mm (6 in.) high.12.2 Mechanical Stirrer, agitator as shown in Fig. 12, attached to a variable-speed motor capable of 1500 r/min.12.3 A constant-temperature bath, set at 25C and capable of maintaining that temperature to within 60.5C.12.4 Water Bath, constant-temperat
32、ure, set at 25C and capable of maintaining that temperature to within 60.5C.13. ProcedurePreparation of the Test Specimen13.1 Determine the moisture in accordance with Sections4 9.13.2 Calculate the sample mass, S, in grams necessary to make 250 g of test solution as follows:S 5 A 31001002B (2)where
33、: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 as follows:W 52502S (3)where:S = sample mass, g.FIG. 12 Stainless Steel AgitatorD5400 15413.4 Weigh the water into the glass bottle and place it on the stirrer, mi
34、xing at a speed sufficient to cause a vortex but not fastenough to splash.13.5 Sprinkle the hydroxypropylcellulose sample into the water slowly, to prevent lumping. Increase stirring speed toapproximately 900 6 100 r/min and stir until the sample is completely dissolved (1 to 2 h).13.6 Remove the gl
35、ass bottle from the stirrer, cap the bottle, and place it in the constant temperature bath for 30 min or as longas necessary to bring the solution to 25 6 0.5C.13.7 Remove the glass bottle from the water bath and invert it slowly 4 to 5 times, taking care to minimize the introduction ofair bubbles.1
36、3.8 Measure the viscosity with the Brookfield viscometer, following the manufacturers operating instructions. Select theproper spindle and speed from Table 1. Allow the spindle to rotate for 3 min before taking the reading. Use the spindle guard.NOTE 1If the room temperature is considerably greater
37、or less than 25C; the entire operation of stirring, standing, and measurement should beconducted with the glass bottle suspended in the constant temperature bath.14. Calculation14.1 Calculate the viscosity, V, in centipoises as follows:V 5r 3f (4)where:r = scale reading andf = factor from Table 1.14
38、. Procedure14.1 Select the appropriate rotational element so that the torque reading is near the midpoint of the scale at a rotational speedbetween 30 and 60 r/min for the viscosity of the test specimen.14.2 Allow the element to rotate for 3 to 4 min before taking a reading.14.3 Measure and report t
39、he viscosity with the rotational viscometer, following the manufacturers operating instructions.NOTE 4If the room temperature is considerably greater or less than 25C; the entire operation of stirring, standing, and measurement should beconducted with the glass bottle suspended in the constant tempe
40、rature bath.15. Report15.1 Report the following information:15.1.1 Results, as Brookfieldapparent viscosity in mPa(cP) at 25C,15.1.2 Solution concentration,15.1.3 Spindle used, andA complete description of the viscometer including manufacturer, model number, rotational element,and rotational speed a
41、nd temperature used.15.1.4 Speed used.16. Precision and Bias16.1 PrecisionStatistical analysis of interlaboratory test results indicates a precision of 610 % at the 95 % confidence level.16.2 BiasNo justifiable statement on bias can be made as no suitable reference material is available as a standar
42、d.pH17. Scope17.1 This test method covers the determination of the pH of aqueous solutions of hydroxypropylcellulose.18. Significance and Use18.1 This test method determines the relative acidity or alkalinity of aqueous solutions of hydroxypropylcellulose. This mustbe taken into consideration when d
43、etermining materials of construction for equipment and packaging for handling and storing thesesolutions. Also, pH may affect suitability for certain end-use applications.19. Apparatus19.1 pH Meter, with glass electrodes.20. Procedure20.1 Determine the pH of the viscosity solution from 13.5, using a
44、 suitable pH meter that has been standardized according toTest Method E70.D5400 15521. Precision and Bias21.1 PrecisionStatistical analysis of intralaboratory test results on samples with pH values of 4.5 to 8.5 indicates a precisionof 65 % at the 95 % confidence level.21.2 BiasNo justifiable statem
45、ent on bias can be made as no suitable reference material is available as a standard.RESIDUE ON IGNITION22. Scope22.1 This test method covers the determination of the amount of residue left from igniting a sample of hydroxypropylcelluloseafter being moistened first with sulfuric acid and then with h
46、ydrofluoric acid.23. Significance and Use23.1 Excessive residue on ignition can affect solution clarity and film properties. The residue on ignition (along with moisture)is a measure of the amount of active polymer in the material and must be considered when determining the amount ofhydroxypropylcel
47、lulose to use in various formulations.23.2 Commercially available hydroxypropylcellulose most often has up to 0.60 % silica added as an anti-caking agent.Therefore, a hydrofluoric acid ashing step is required to remove the silica.24. Apparatus24.1 Dishes, platinum, 75-mL capacity.24.2 Hot Plate.24.3
48、 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, about 1 g of hydroxypropylcellulose into a tared platinum dish. Using a hot plate, heat thedis
49、h containing the sample (gently at first) until the sample is thoroughly charred. Cool the dish for several minutes.26.2 Moisten the residue with about 1 mL of sulfuric acid and heat gently on the hot plate until white fumes are no longerevolved.26.3 Place the dish in a muffle furnace at 800 6 25C for 30 min. Allow the dish to cool.26.4 Repeat 26.2 and 26.3. Cool in a desiccator. Weigh the residue (R1).26.5 Moisten the residue with up to 1 mL of water and carefully add about 5 mL of hydrofluoric acid, in small porti
