1、Designation: D 2364 01 (Reapproved 2007)e1Standard Test Methods forHydroxyethylcellulose1This standard is issued under the fixed designation D 2364; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numbe
2、r in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTESpecification E 1 was replaced with Specification E 2251 in Section 2 and 20.5 in June 2007.1. Scope1.1 These test methods cover the testing of h
3、ydroxyethyl-cellulose.1.2 The test procedures appear in the following order:SectionsMoisture 4-9Ash 10-17Viscosity 18-24Density 25-311.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to estab
4、lish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 4794 Test Method for Determination of Ethoxyl or Hy-droxyethoxyl Substitution in Cellulose Ether Pr
5、oducts byGas ChromatographyE 2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision Liquids3. Purity of Reagents3.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the C
6、ommittee on AnalyticalReagents of the American Chemical Society,3where suchspecifications are available. Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.3.2 Unless otherwis
7、e indicated, reference to water shall beunderstood to mean reagent water, conforming to SpecificationD 1193.MOISTURE4. Scope4.1 This test method covers the determination of the volatilecontent of hydroxyethylcellulose.5. Significance and Use5.1 The results of this test are used for calculating the t
8、otalsolids in the sample; and, by common usage, all materialsvolatile at this test temperature are designated as moisture.5.2 Moisture analysis (along with sulfated ash) is a measureof the amount of active polymer in the material and must beconsidered when determining the amount of hydroxyethylcellu
9、lose to use in various formulations.6. Apparatus6.1 Oven, gravity-convection, capable of maintaining atemperature of 105 6 3C.6.2 Weighing Bottles, low-form, 50 mm in inside diameterby 30 mm in height, or equivalent.6.3 Analytical Balance.7. Procedure7.1 Weigh5gofsample to the nearest 0.001 g in a t
10、ared andcovered weighing bottle.7.2 Place it in an oven at 105C for 2 h with the coverremoved. Replace the cover, cool in a desiccator, and weigh.8. Calculation8.1 Calculate the percent moisture, M, as follows:M 5 A/B! 3 100 (1)1These test methods are under the jurisdiction of ASTM Committee D01 onP
11、aint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved June 1, 2007. Published July 2007. Originally approvedin 1965. Last previous edition approved in 2001 as D 2364 01.2For refer
12、enced 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 Chemical Society Specifications, AmericanC
13、hemical 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. Pharmacopeial Convention, Inc. (USPC), R
14、ockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.where:A = mass loss on heating, g, andB = sample used, g.9. Precision and Bias9.1 Statistical analysis of intralaboratory (repeatability) testresults on samples containing f
15、rom about 3.5 % moistureindicate a precision of 60.5 % absolute at the 95 % confidencelevel.9.2 No statement on bias can be made as no suitablereference material is available as a standard.ASHAS SULFATE10. Scope10.1 This test method covers the determination of theresidue on ignition of hydroxyethylc
16、ellulose after a specimenhas been treated with sulfuric acid.11. Summary of Test Method11.1 A specimen is moistened with sulfuric acid, the excessacid evaporated, the carbonaceous matter burned off, and theresidue ignited in a muffle furnace, cooled, and weighed.12. Significance and Use12.1 Excessiv
17、e ash can affect solution clarity and filmproperties. The ash (along with moisture) is a measure of theamount of active polymer in the material and must be consid-ered when determining the amount of hydroxyethyl cellulose touse in various formulations.13. Apparatus13.1 Dishes, platinum, 50 to 75-mL
18、capacity.13.2 Muffle Furnace, maintained at 825 6 25C.14. Reagents14.1 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric acid(H2SO4).15. Procedure15.1 Weigh, to the nearest 0.0001 g, about2gofthedriedsample into a tared platinum dish. Moisten the entire specimenwith about 2 mL of H2SO4. Then cautiousl
19、y heat over a smallflame until sulfur trioxide (SO3) fumes cease to be evolved.15.2 Increase the heat, ignite the specimen, and heat asnecessary to burn off the volatile matter. Avoid spattering.15.3 Place the dish in a 825C muffle furnace for 1 h, orlonger if required, to burn all of the carbon.15.
20、4 Remove the dish, allow to cool somewhat, place in adesiccator, and cool to room temperature. Weigh the dish andresidue to the nearest 0.0001 g.16. Calculation16.1 Calculate the percent of ash (as sulfate), C, as follows:C 5 A/B!3 100 (2)where:A = ash, g, andB = sample used, g.17. Precision and Bia
21、s17.1 Statistical analysis of interlaboratory (reproducibility)test results on samples containing 2 to 5 % ash (as sulfate)indicates a precision of 60.3 % absolute at the 95 % level.17.2 No statement on bias can be made as no suitablereference material is available as a standard.VISCOSITY18. Scope18
22、.1 This test method is an arbitrary method of determiningthe viscosity of aqueous solutions of hydroxyethylcellulose inthe viscosity range from 10 to 10 000 cP at 25C.18.2 The concentration to be used for the test shall beagreed upon between the purchaser and the seller. It shall besuch that the vis
23、cosity of the solution will fall within the rangeof this test.18.3 The results for the viscosity of hydroxyethylcelluloseby this test method will not necessarily check with results fromother types of instruments used for viscosity measurements.18.4 The determinations are run on a calculated dry basi
24、s;that is, the amount of hydroxyethylcellulose required for thedesired concentration on a dry basis is calculated from theknown moisture content.19. Significance and Use19.1 This test method is intended for referee purposes. TheBrookfield spindles and speeds given in Table 1 are recom-mended for thi
25、s purpose, but slight deviations from Table 1may occasionally be found convenient for individual applica-tion.19.2 This test method determines the relative ability of thepolymer to thicken aqueous solutions and is therefore related tothe concentration required in various formulations to achievethe d
26、esired finished product viscosity.20. Apparatus20.1 Viscometer, Rotational type.NOTE 1Manufacturers of cellulose derivatives usually specify theviscometer make, model, spindle, and speed to be used with theirproducts. It is highly recommended that these specifications be followed.Use of a viscometer
27、 made by another company or even a different modelby the same company will result in slightly different results.20.2 Container, glass jar, 350-cm3approximately 64 mm inoutside diameter and 152 mm high.TABLE 1 Viscometer Spindles Required for Given SpeedsViscosity Range,cPSpindle No. Speed, rpm Scale
28、 Factor10 to 100 1 60 100 1100 to 200 1 30 100 2200 to 1000 2 30 100 101000 to 4000 3 30 100 404000 to 10 000 4 30 100 200D 2364 01 (2007)e1220.3 Mechanical StirrerAgitator as shown in Fig. 1 orFig. 2,4attached to a variable-speed motor capable of 1500r/min.20.4 Water Bath, constant-temperature, set
29、 at 25C andcapable of maintaining that temperature to within 60.2C.20.5 ThermometerAn ASTM Saybolt Viscosity Ther-mometer having a range from 19 to 27C and conforming tothe requirements for Thermometer 17C, as prescribed inSpecification E 2251.21. Procedure21.1 Determine the moisture in accordance w
30、ith Sections4-9.21.2 Calculate the dry-basis specimen mass, M, in gramsnecessary to make 250 g of test solution as follows:Ms5 100 A/100 B! (3)where:A = desired dry mass of specimen, g, andB = percent moisture in the weighed specimen.21.3 Add the specimen to the jar. Then add sufficientdistilled wat
31、er to make a total of 250 g of solution. Calculatethe mass of water, MW, in grams as follows:Mw5 250 S (4)where S = sample mass, g.4An agitator made with 112 in. (38 mm), three-bladed propellers has been foundsatisfactory for this purpose.in. mm in. mm116 1.5516 7.9316 4.858 15.814 6.4 112 38932 791
32、2 241FIG. 1 AgitatorFIG. 2 AgitatorD 2364 01 (2007)e1321.4 Place the agitator in the solution allowing a minimumclearance between the agitator and the bottom of the container.Stir at approximately 1500 r/min until the specimen is com-pletely dissolved. This may require several hours.21.5 Remove the
33、agitator from the motor and transfer thespecimen container, with the agitator in it, to the constanttemperature bath. Allow it to stand for 1 h.21.6 Remove the specimen container from the bath andshake or stir vigorously for 10 s. Measure the viscosity with therotational viscometer, following the ma
34、nufacturers instruc-tions, selecting the proper spindle and speed from Table 1.Allow the spindle to rotate for 3 min before taking a reading.NOTE 2If the room temperature is considerably greater or less than25C, the entire operation of stirring, standing, and measurement shouldbe conducted with the
35、specimen suspended in the water bath.21.6.1 Warning Shaking or stirring the sample maycause entrainment of air bubbles. One must exercise care toavoid having a large air bubble under the viscometer spindlewhen taking the measurement.22. Calculation22.1 Calculate the viscosity, V, in centipoises as f
36、ollows:V 5 r 3 f (5)where:r = reading andf = factor.23. Report23.1 Report the following information:23.1.1 Results, as viscosity at 25C,23.1.2 Solution concentration,23.1.3 Spindle used, and23.1.4 Speed used.24. Precision and Bias24.1 PrecisionStatistical analysis of interlaboratory (re-producibilit
37、y) test results indicates a precision of 610 % at the95 % confidence level when using the same viscometer makeand model.24.2 BiasNo justifiable statement can be made on the biasof the procedure for measuring viscosity because no suitablereference material exists.DENSITY25. Scope25.1 This test method
38、 covers the determination of the bulkdensity of hydroxyethylcellulose.26. Summary of Test Method26.1 A weighed amount of hydroxyethylcellulose is trans-ferred to a 100-mL graduated cylinder and the graduatevibrated to settle the powder.27. Significance and Use27.1 Density can relate to dry flow prop
39、erties, rate ofdissolution, lumping, packaging, and storage space require-ments.28. Apparatus28.1 VibratorA magnetic-type electric vibrator attachedto the vertical support rod of a ring stand approximately 0.3 mabove the base. A condenser clamp of sufficient size to hold a100-mL graduated cylinder a
40、lso shall be attached to the aboverod. The base of the stand should be weighted.29. Procedure29.1 Place 50.0 g of hydroxyethylcellulose in a 100-mLgraduated cylinder and place in the condenser clamp. Turn onthe vibrator and allow the cylinder to vibrate for 3 min. Recordthe level (in millilitres) to
41、 which the specimen has compacted.29.2 Alternatively, the specimen may be compacted manu-ally. Tap it on a hard surface by dropping the cylinderrepeatedly from a height of about 25 mm until the volume ofthe sample remains constant. In order to prevent cylinderbreakage, cover the tapping surface with
42、a3to6-mm thickrubber sheet, or use a plastic graduated cylinder.30. Calculation30.1 Calculate the density, D, in grams per millilitre asfollows:D 5 50/ro(6)where Ro= observed reading, mL.31. Precision and Bias31.1 PrecisionStatistical analysis of intralaboratory (re-peatability) test results indicat
43、es a precision of 60.04 g/mL atthe 95 % confidence level.31.2 BiasNo justifiable statement on the bias of theprocedure for measuring density can be made because nosuitable reference material exists.MOLAR SUBSTITUTION: see Test Method D 479432. Keywords32.1 ash; density; hydroxyethylcellulose; moistu
44、re; molarsubstitution; viscosityD 2364 01 (2007)e14ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent righ
45、ts, 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
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47、you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 2364 01 (2007)e15
