1、Designation: D2364 01 (Reapproved 2007)1D2364 15Standard Test Methods forHydroxyethylcellulose1This standard is issued under the fixed designation D2364; 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 NOTESpecification E 1 was replaced with Specification E 2251 in Section 2 and 20.5 in June 2007.1. Scope Scope*1.1 These test methods cover the t
3、esting of hydroxyethylcellulose.1.2 The test procedures appear in the following order:SectionsMoisture 4 9Ash 10 17Viscosity 18 24Viscosity 18 23Density 25 31Density 24 301.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.
4、4 This standard does not purport to address all of the safety concerns, if any, associated 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.2. Referenced Docum
5、ents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD4794 Test Method for Determination of Ethoxyl or Hydroxyethoxyl Substitution in Cellulose Ether Products by GasChromatographyE2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids3. Purity of Reagents3
6、.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society,3 where such specifications areavailable. Other grades may be used, provided
7、 it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.3.2 Unless otherwise indicated, reference to water shall be understood to mean reagent water, conforming to SpecificationD1193.MOISTURE4. Scope4.1 This test m
8、ethod covers the determination of the volatile content of hydroxyethylcellulose.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 Derivati
9、ves.Current edition approved June 1, 2007Dec. 1, 2015. Published July 2007April 2016. Originally approved in 1965. Last previous edition approved in 20012007 asD2364 01.D2364 01 (2007)1. DOI: 10.1520/D2364-01R07E01.10.1520/D2364-15.2 For referencedASTM standards, visit theASTM website, www.astm.org,
10、 or 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 Suggestion
11、s 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 stan
12、dard 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 case
13、s 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 States15. Significance
14、and Use5.1 The results of this 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 sulfated ash) is a measure of the amount of active polymer in the material an
15、d must beconsidered when determining the amount of hydroxyethyl cellulose to use in various formulations.6. Apparatus6.1 Oven, gravity-convection, capable of maintaining a temperature of 105 6 3C.6.2 Weighing Bottles, low-form, 50 mm in inside diameter by 30 mm in height, or equivalent.6.3 Analytica
16、l Balance.7. Procedure7.1 Weigh 5 g of sample to the nearest 0.001 g in a tared and covered weighing bottle.7.2 Place it in an oven at 105C for 2 h with the cover removed. Replace the cover, cool in a desiccator, and weigh.8. Calculation8.1 Calculate the percent moisture, M, as follows:M 5A/B!3100 (
17、1)where:A = mass loss on heating, g, andB = sample used, g.9. Precision and Bias9.1 Statistical analysis of intralaboratory (repeatability) test results on samples containing from about 3.5 % moisture indicatea precision of 60.5 % absolute at the 95 % confidence level.9.2 No statement on bias can be
18、 made as no suitable reference material is available as a standard.ASHAS SULFATE10. Scope10.1 This test method covers the determination of the residue on ignition of hydroxyethylcellulose after a specimen has beentreated with sulfuric acid.11. Summary of Test Method11.1 Aspecimen is moistened with s
19、ulfuric acid, the excess acid evaporated, the carbonaceous matter burned off, and the residueignited in a muffle furnace, cooled, and weighed.12. Significance and Use12.1 Excessive ash can affect solution clarity and film properties. The ash (along with moisture) is a measure of the amount ofactive
20、polymer in the material and must be considered when determining the amount of hydroxyethyl cellulose to use in variousformulations.13. Apparatus13.1 Dishes, platinum, 50 to 75-mL capacity.13.2 Muffle Furnace, maintained at 825 6 25C.14. Reagents14.1 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric ac
21、id (H2SO4).15. Procedure15.1 Weigh, to the nearest 0.0001 g, about 2 g of the dried sample into a tared platinum dish. Moisten the entire specimen withabout 2 mL of H2SO4. Then cautiously heat over a small flame until sulfur trioxide (SO3) fumes cease to be evolved.15.2 Increase the heat, ignite the
22、 specimen, and heat as necessary to burn off the volatile matter. Avoid spattering.15.3 Place the dish in a 825C muffle furnace for 1 h, or longer if required, to burn all of the carbon.D2364 15215.4 Remove the dish, allow to cool somewhat, place in a desiccator, and cool to room temperature. Weigh
23、the dish and residueto the nearest 0.0001 g.16. Calculation16.1 Calculate the percent of ash (as sulfate), C, as follows:C 5A/B!3100 (2)where:A = ash, g, andB = sample used, g.17. Precision and Bias17.1 Statistical analysis of interlaboratory (reproducibility) test results on samples containing 2 to
24、 5 % ash (as sulfate) indicatesa precision of 60.3 % absolute at the 95 % level.17.2 No statement on bias can be made as no suitable reference material is available as a standard.VISCOSITY18. Scope18.1 This test method is an arbitrary method of determining the viscosity of aqueous solutions of hydro
25、xyethylcellulose in theviscosity range from 10 to 10 000 cP mPas (cP) at 25C.18.2 The concentration to be used 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.18.3 The results for the v
26、iscosity of hydroxyethylcellulose by this test method will not necessarily checkagree with results fromother types of instruments used for viscosity measurements.18.4 The determinations are run on a calculated dry basis; that is, the amount of hydroxyethylcellulose required for the desiredconcentrat
27、ion on a dry basis is calculated from the known moisture content.19. Significance and Use19.1 This test method is intended for referee purposes. The Brookfield spindles and speeds given in Table 1 are recommendedfor this purpose, but slight deviations from may occasionally be found convenient for in
28、dividual application.19.2 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.FIG. 1 Coaxial Cylinder Rotational ElementD2364 15320
29、. Apparatus20.1 Viscometer, Coaxial RotationalRotational type.The essential instrumentation required providing the minimum rotationalviscometer analytical capabilities for this method include:NOTE 1Manufacturers of cellulose derivatives usually specify the viscometer make, model, spindle, and speed
30、to be used with their products. It ishighly recommended that these specifications be followed. Use of a viscometer made by another company or even a different model by the same companywillmay result in slightly different results.20.1.1 A drive motor to apply a unidirectional rotational displacement
31、to the specimen at a rate from 0.5 to 60 r/min constantto within 61 %.20.1.2 Aforce sensor to measure the torque developed by the specimen to the rotational displacement of the rotational element.20.1.3 A coupling shaft or other means to transmit the rotational displacement from the motor to the spe
32、cimen.20.1.4 A rotational element, spindle, or tool to fix the specimen between the drive shaft and a stationary position.NOTE 2Each rotational element typically covers a range of about 2 decades of viscosity. The rotational element is selected so that the measuredviscosity is between 10 and 90 % of
33、 the range of that rotational element.NOTE 3Coaxial cylinder rotational elements of the form shown inFig. 1 are suitable for this standard.20.1.5 A specimen container, approximately 64 mm in outside diameter, 152 mm in height, and 350 mL in volume, to containthe test specimen during testing.20.1.6 A
34、data collection device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.The minimum output signals required for rotational viscometry are torque, rotational speed, temperature, and time.20.1.7 A stand, to support, level, and adjust the height of the d
35、rive motor, shaft, and rotational element.20.1.8 Auxiliary instrumentation considered necessary or useful in conducting this method includes:20.1.8.1 Data analysis capability to provide viscosity, stress or other useful parameters derived from the measured signals.20.1.8.2 A level to indicate the ve
36、rtical plumb of the drive motor, shaft and rotational element.20.2 Container, glass jar, 350-cm3 approximately 64 mm in outside diameter and 152 mm high.20.2 Mechanical StirrerAgitator as shown in Fig. 12 or Fig. 23, attached to a variable-speed motor capable of 1500r/min.r/min rotational speed.NOTE
37、 4An agitator made with 38 mm (1.5 in) three-bladed propellers is satisfactory for this purpose.20.3 Water Bath, constant-temperature, set at 25C and capable of maintaining that temperature to within 60.2C.20.4 ThermometerAnAASTM Saybolttemperature sensorViscosityThermometer having a range fromto pr
38、ovide an indicationof the specimen temperature over the range of 19 to 27C and conforming to the requirements for Thermometer 17C, as prescribedin Specification to within 60.1C.E2251.21. Procedure21.1 Determine the moisture in accordance with Sections4 9.21.2 Calculate the dry-basis specimen mass, M
39、, in grams necessary to make 250 g of test solution as follows:Ms 5100 A/1002B! (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 sufficient distilled water to make a total of 250 g of solution. Calculate the mass
40、of water, MW, in grams as follows:Mw 52502S (4)where:S = sample mass, g.where S = sample mass, g.21.4 Place the agitator in the solution allowing a minimum clearance between the agitator and the bottom of the container. Stirat approximately 1500 r/min until the specimen is completely dissolved. This
41、 may require several hours.21.5 Remove the agitator from the motor and transfer the specimen container, with the agitator in it, to the constant temperaturebath. Allow it to stand for 1 h.D2364 15421.6 Remove the specimen container from the bath and shake or stir vigorously for 10 s. Measure the vis
42、cosity with therotational viscometer, following the manufacturers instructions, selecting the proper spindle and speed from Table 1. Allow thespindle to rotate for 3 min before taking a reading.NOTE 5If the room temperature is considerably greater or less than 25C, the entire operation of stirring,
43、standing, and measurement should beconducted with the specimen suspended in the water bath.21.6.1 WarningShaking or stirring the sample may cause entrainment of air bubbles. One must exercise care to avoid havinga large air bubble under the viscometer spindle when taking the measurement.in. mm in. m
44、m116 1.5 516 7.9316 4.8 58 15.814 6.4 112 38932 7 912 241FIG. 1 AgitatorFIG. 2 AgitatorD2364 15521.7 Measure the viscosity with the rotational viscometer at a rotational speed of 30 or 60 r/min using a coaxial spindle (seeFig. 1) suitable for the test specimen viscosity. Allow the spindle to rotate
45、for 3 min before taking a reading.21.7.1 WarningShaking or stirring the sample may cause entrainment of air bubbles. One must exercise care to avoid havinga large air bubble under the viscometer spindle when taking the measurement.22. Calculation22.1 Calculate the viscosity, V, in centipoises as fol
46、lows:V 5r 3f (5)where:r = reading andf = factor.22. Report22.1 Report the following information:22.1.1 Results, as viscosity Viscosity at 25C,22.1.2 Solution concentration,22.1.3 Spindle used, andComplete description of the apparatus used including manufacturer, model number and spindle, and22.1.4 S
47、peed Description of experimental conditions including rotational speed used.23. Precision and Bias23.1 PrecisionStatistical analysis of interlaboratory (reproducibility) test results indicates a precision of 610 % at the 95 %confidence level when using the same viscometer make and model.23.2 BiasBia
48、sNoNo justifiable statement can be made on the bias of the procedure for measuring viscosity because nosuitable reference material exists.FIG. 3 AgitatorD2364 156DENSITY24. Scope24.1 This test method covers the determination of the bulk density of hydroxyethylcellulose.25. Summary of Test Method25.1
49、 A weighed amount of hydroxyethylcellulose is transferred to a 100-mL graduated cylinder and the graduate vibrated tosettle the powder.26. Significance and Use26.1 Density can relate to dry flow properties, rate of dissolution, lumping, packaging, and storage space requirements.27. Apparatus27.1 VibratorAmagnetic-type electric vibrator attached to the vertical support rod of a ring stand approximately 0.3 m abovethe base. A condenser clamp of sufficient size to hold a 100-mL graduated cylinder also shall be attac
